JP7386538B2 - Cooks, reaction equipment, and chemical product manufacturing methods - Google Patents

Description

The present disclosure relates to a seal member, a cock, a reaction device, and a method for manufacturing a chemical product.

When conducting experiments using chemical substances or manufacturing chemical products, it may be necessary to prevent air from entering the reactor in order to reduce by-products, suppress decomposition of reaction products, and the like. In such cases, for example, it is possible to place the reactor in a glove box filled with inert gas as described in Patent Document 1, and supply raw materials and perform various operations therein. It becomes necessary. When working with such a glove box, it is necessary to wear gloves that are directly connected to the box.

JP2013-240850A

Since work inside a glove box requires wearing gloves, it is difficult to perform detailed operations with the hands, which places a burden on the worker. Furthermore, it is necessary to install experimental equipment or manufacturing equipment in the glove box and then replace the inside of the glove box with an inert gas. For this reason, preparation requires time and effort, resulting in a decrease in work efficiency. Therefore, the present disclosure provides a seal member, a cock, and a reaction device that can improve work efficiency when handling chemical substances. The present invention also provides a method for manufacturing chemical products that can efficiently manufacture chemical products.

A sealing member according to one aspect of the present disclosure is a sealing member provided between at least two tubes, and has a holding portion that holds a sample, and moves the sample from one tube side to the other tube side. configured as possible. Such a sealing member has a simple configuration and can move a sample while maintaining sealing properties, and thus can improve work efficiency when handling chemical substances.

The holder is composed of a recess that accommodates the sample, and the recess may rotate to move the sample from one tube side to the other tube side. By having a recess for accommodating a sample, the amount of sample that can be held and moved can be increased.

The sealing member is rotatably attached to the cock body that connects the at least two pipe bodies, and has a sliding part that slides against the inner wall surface of the cock body, and the holding part is defined by the sliding part. may be provided within the area. By having such a sliding portion, the sealing performance of the sealing member can be made sufficiently excellent.

The sealing member may be slidably attached to the cock body connecting the at least two tubes. This allows the sample to be moved with a simple operation. The sealing member may slide with respect to the cock body so that a state in which the holding portion communicates with the flow path of one tube and a state in which the holding portion communicates with the other tube are switched.

A sealing member according to one aspect of the present disclosure is a sealing member provided between at least two tubes, and is slidably attached to a cock body connecting the at least two tubes, and the sealing member is provided between at least two tubes. The penetrating through hole and the inner wall surface of the cock body that connects the two tubes constitute a holding section that holds the sample, and the sample is configured to be movable from one tube side to the other tube side. Such a sealing member has a simple configuration and can move a sample while maintaining sealing properties, and thus can improve work efficiency when handling chemical substances.

The at least two tubes may include a first tube and a second tube. In this case, the sealing member may be configured to be able to move the sample from the first tube side to the second tube side without communicating the first tube body and the second tube body. Thereby, the first tube body and the second tube body can be sufficiently isolated.

A seal member according to one aspect of the present disclosure is a seal member rotatably attached to a cock body, and includes a sliding portion that slides against an inner wall surface of the cock body during rotation; a recess formed within a region defined by the recess, which is configured to be able to hold and release a sample by rotating with rotation.

Such a seal member has a simple configuration and can hold and release a sample by a simple operation of rotating the seal member. Further, since the recessed portion is formed within the area defined by the sliding portion, the sealing performance is sufficiently excellent. Therefore, work efficiency when handling chemical substances can be improved.

A cock according to one aspect of the present disclosure includes at least two pipe bodies, a cock body that connects them, and any of the above-mentioned seal members attached to the cock body. This cock has a simple configuration and is equipped with a sealing member that can hold and release a sample while having sealing properties, and thus can improve work efficiency when handling chemical substances.

A reaction device according to one aspect of the present disclosure includes the sealing member and a reactor, and a sample falls into the reactor from the holding part. This reaction apparatus allows the sample held in the holding section to fall into the reactor. Since such a reaction device has a simple configuration and allows a sample to fall into the reactor while maintaining sealing properties, it is possible to improve work efficiency when handling chemical substances.

A reaction device according to one aspect of the present disclosure includes a seal member and a reactor, and a sample falls into the reactor from the recess. This reaction device allows the sample held in the recess to fall into the reactor. Since such a reaction device has a simple configuration and allows a sample to fall into the reactor while maintaining sealing properties, it is possible to improve work efficiency when handling chemical substances.

A method for manufacturing a chemical product according to one aspect of the present disclosure includes a step of manufacturing a chemical product using the above-mentioned reaction device. Since this manufacturing method uses the above-mentioned reaction apparatus, chemical products can be efficiently manufactured.

According to the present disclosure, it is possible to provide a seal member, a cock, and a reaction device that can improve work efficiency when handling chemical substances. Furthermore, it is possible to provide a method for manufacturing chemical products that can efficiently manufacture chemical products.

It is a figure showing a seal member and a cock concerning a 1st embodiment. It is a figure showing a seal member and a cock concerning a 1st embodiment. FIG. 2 is an exploded view of the cock according to the first embodiment. FIG. 1 is a diagram of a reaction apparatus according to a first embodiment. It is a figure which shows the sealing member based on 2nd Embodiment. It is a figure showing a seal member and a cock concerning a 3rd embodiment. It is a figure showing a seal member and a cock concerning a 3rd embodiment. It is a figure showing a seal member and a cock concerning a 3rd embodiment. It is a figure which shows the seal member and cock based on 4th Embodiment. It is a figure which shows the seal member and cock based on 4th Embodiment.

Hereinafter, some embodiments of the present disclosure will be described with reference to the drawings, as the case may be. However, each embodiment below is an illustration for explaining the present disclosure, and is not intended to limit the present disclosure to the following content. In the description, the same reference numerals will be used for the same elements or elements having the same function, and redundant description will be omitted in some cases. In addition, the positional relationships such as top, bottom, left, and right are based on the positional relationships shown in the drawings unless otherwise specified. Furthermore, the dimensional ratio of each element is not limited to the ratio shown in the drawings.

FIG. 1 is a diagram showing a seal member and a cock according to the first embodiment. The cock 60 in FIG. 1 includes a cock body 40, a first tube 20 and a second tube 30 that are connected to the cock body 40, sandwiching the cock body 40 from above and below, for example, and the cock body 40. The sealing member 10 is inserted into and blocks the first tubular body 20 and the second tubular body 30. The sealing member 10 has a sealing function of suppressing gas intrusion, a function of holding a sample, and a function of moving the sample from the first tube body 20 side to the second tube body 30 side.

The seal member 10 has a handle portion 14 at one end, a fixed portion 16 at the other end, and a sliding portion 18 between both ends. The seal member 10 is restricted from moving in the lateral direction in FIG. 1 by the handle portion 14 and the fixing portion 16, and is rotatably fixed to the cock body portion 40. The fixing portion 16 is threadedly engaged with the fixing member 52 via the packing 50, and the sealing member 10 rotates with respect to the cock body 40 together with the packing 50 and the fixing member 52.

When the seal member 10 rotates relative to the cock body 40 , the sliding portion 18 of the seal member 10 slides against the inner wall surface 42 of the cock body 40 . The recess 12 is defined by a sliding portion 18, and the sealing member 10 rotates while the sliding portion 18 slides against the inner wall surface 42. Therefore, even while the seal member 10 is being rotated with respect to the cock body 40, the cock 60 can maintain good sealing performance. For example, it is possible to prevent gas from flowing into the second pipe 30 from the first pipe 20 and to prevent outside air from entering through the gap between the cock body 40 and the seal member 10.

As shown in FIG. 1, if a sample is introduced from the first tube 20 while the recess 12 is exposed to the flow path of the first tube 20, the sample is retained in the recess 12. The recess 12 may be formed in, for example, a mortar shape, a funnel shape, or a hemispherical shape so as to expand in a direction from the rotation axis of the sealing member 10 toward the circumferential surface, from the viewpoint of sufficiently smoothing the accommodation and discharge of the sample. The outer edge of the recess 12 may be angular in order to prevent the sample from entering between the sliding portion 18 and the inner wall surface 42 .

FIG. 2 is a diagram showing the same cock 60 as FIG. 1, but shows a state different from that shown in FIG. FIG. 2 shows a state in which the seal member 10 is rotated half a turn from the state shown in FIG. The seal member 10 can be rotated by operating the handle portion 14. When the sealing member 10 is rotated from the state shown in FIG. 1, the fixing member 52 and the packing 50 may also be rotated together. At this time, the packing 50 may rotate while sliding on the end surface of the cock body 40.

When the seal member 10 is rotated half a turn with respect to the cock body 40, the recess 12 rotates with the rotation of the seal member 10 and is exposed to the flow path of the second tube body 30. As shown in FIGS. 1 and 2, when the second tube 30 is located lower than the first tube 20, when the state shown in FIG. 2 is reached, the sample that was accommodated in the recess 12 in the state shown in FIG. , after turning, it falls in the flow path of the second tube body 30 due to gravity. In this way, the cock 60 can discharge the sample from the recess 12 using gravity, so the sample can be introduced into a reactor or the like connected below the second tube 30 with an extremely simple operation.

After the sample is dropped from the recess 12 in the state shown in FIG. 2, when the seal member 10 is further rotated by half a turn with respect to the cock body 40, the state shown in FIG. 1 is returned. In this state, the sample may be introduced into the recess 12 again via the flow path of the first tube 20. In this way, the recess 12 corresponding to the sample holding section can repeatedly accommodate (hold) and release the sample.

The seal member 10 does not have a through hole that allows the first tube body 20 and the second tube body 30 to communicate with each other. Therefore, it is possible to suppress the flow of a medium such as gas between the first tube 20 and the second tube 30. Further, the sealing member 10 has a sliding portion 18 that slides on the inner wall surface 42 of the cock body 40 during rotation, thereby continuously sealing the flow path of the second tube 30. That is, the recessed portion 12 is surrounded by the sliding portion 18 and is formed within a region defined by the sliding portion 18 . Therefore, even when the recess 12 is exposed to the flow path of the second tube body 30, since the inner wall surface 42 of the cock body 40 and the sliding part 18 are in contact with each other, both ends of the cock body 40 are exposed. Intrusion of outside air into the flow path of the second pipe body 30 can be sufficiently suppressed.

The cock 60 allows a sample to be introduced into the recess 12 in the state shown in FIG. 1, and discharges the sample from the recess 12 in the state shown in FIG. Even while operating the handle portion 14 to change the state from the state shown in FIG. 1 to the state shown in FIG. . In this way, the cock 60 is excellent not only in airtightness but also in blocking performance between the first tube body 20 and the second tube body 30. Therefore, the cock 60 is particularly useful as a sample supply device for a reaction device that requires high airtightness and high barrier properties.

The sample may be a liquid sample or a solid sample. There is no particular restriction on the type of sample, and it may be an organic substance, an inorganic substance, or a mixture thereof. For example, it may be a sample used as a raw material for an organic synthesis reaction where it is necessary to sufficiently suppress the intrusion of air and moisture. As a result, various organic compounds such as organic materials, medicines, and agricultural chemicals can be efficiently produced.

If the sample is a liquid, it can be introduced into the reactor in a gas-tight manner, for example by cannulation. However, if the sample is solid, it cannot be introduced by cannulation. Therefore, the seal member 10 and the cock 60 of this embodiment are particularly useful when it is necessary to introduce a sample that does not dissolve in a solvent or a sample that is difficult to dissolve in a solvent. In addition, in the case of cannulation, it may be necessary to use a solvent unnecessary for the reaction, but the cock of this embodiment has the advantage that the sample can be introduced without using a solvent unnecessary for the reaction. has an advantage.

FIG. 3 is an exploded view of the cock 60. A sliding portion 18 between the handle portion 14 and the fixed portion 16 of the seal member 10 is tapered so as to become thinner from the handle portion 14 toward the fixed portion 16. The seal member 10 is inserted into the cock body 40 and the packing 50, and is rotatably attached to the cock body 40 by screwing the fixing part 16 and the fixing member 52 together. The method of fixing the seal member 10 to the cock body 40 is not limited to this method, and any method that allows for rotatable fixation can be adopted as appropriate.

The seal member 10 may be made of resin, glass, or metal, for example. From the viewpoint of improved sealing performance and corrosion resistance, it may be made of resin or glass. Furthermore, from the viewpoint of ease of processing or slidability, it may be made of resin. The resin may be a fluororesin from the viewpoint of improving durability. When the sealing member 10 is made of glass, at least the sliding portion 18 may be made of frosted glass or resin from the viewpoint of improving airtightness and operability. The cock body portion 40 may be made of glass, resin, or metal.

FIG. 4 is a diagram showing a reaction apparatus according to the first embodiment. The reaction apparatus 100 includes a reactor 70 and a cock 60 connected to the reactor 70. The reactor 70 may be, for example, a glass flask including a main pipe 71 and a side pipe 72. The cock 60 is arranged such that the first tube 20 is above the cock body 40 and the second tube 30 is below the cock body 40. It is inserted into the main pipe 71 of. A removable stopper 86 is attached to the opening of the first tube 20. By removing the stopper 86 and introducing the sample through the opening of the first tube 20, the sample can be accommodated in the recess of the seal member 10 provided in the cock 60.

A valve 74 is connected to the side pipe 72 of the reactor 70 . A needle 84 communicating with a manifold 82 passes through and is connected to a cap 76 attached to the tip of the valve 74 . By operating the valve 74, an inert gas such as argon gas can be supplied from the manifold 82 into the reactor 70, or the pressure inside the reactor 70 can be reduced.

A refrigerant 90 containing dry ice is stored in a temperature adjustment tank 95 equipped with a stirring function, and at least a portion of the reactor 70 is immersed in the refrigerant 90 . When a magnetic stirrer is placed in the reactor 70 together with the raw material liquid 110 and the stirring function is activated, the raw material liquid 110 is stirred and cooled to a desired temperature range by heat exchange with the refrigerant 90. When the handle portion 14 of the cock 60 is operated with the interior of the reactor 70 replaced with an inert gas, the sample contained in the recess 12 is transferred into the reactor 70 via the second tube 30. It falls and is mixed with the raw material liquid 110.

In this way, the sample can be introduced into the reactor 70 simply by operating the handle portion 14. Further, the cock 60 can sufficiently suppress the intrusion of outside air into the second tube 30 while blocking the first tube 20 and the second tube 30 from each other. Since the sealing property is excellent in this way, the sample can be introduced into the reactor 70 with a simple operation while sufficiently suppressing the intrusion of outside air into the reactor 70. Therefore, it is particularly effective when performing reactions that require airtightness.

The reactor of the present disclosure is not limited to the embodiments described above. The refrigerant may be ice water or liquid nitrogen. The temperature control tank 95 may be an oil bath, and in this case, the reactor 70 may be heated and the reaction may be carried out under heated reflux. The reactor 70 may be a glass-lined reactor instead of a flask. In that case, the reactor may be of a jacket type so that it can be heated with steam or the like.

FIG. 5 is a diagram showing a sealing member according to a second embodiment of the present disclosure. The sealing member 10B in FIG. 5 includes a shutter portion 12A, and is provided between the first tube 20 and the second tube 30. The shutter section 12A has both the function of a sample holding section and the function of blocking the first tube 20 and the second tube 30. If a sample is introduced from the first tube body 20 with the shutter section 12A closed, the sample is held on the shutter section 12A. Then, when the lever 17 is operated to open the shutter section 12A, the sample moves from the first tube 20 side to the second tube 30 side and is discharged into the flow path of the second tube 30.

The sample discharged into the flow path of the second tube 30 is introduced into a reactor connected below the second tube 30, for example. After that, if the shutter section 12A is closed, the shutter section 12A can repeatedly hold and release the sample. In this embodiment, the sample can be held and released only by opening and closing the shutter section 12A. Since the sample can be held and moved with such a simple configuration, work efficiency when handling chemical substances can be improved.

6 to 8 are diagrams showing a seal member and a cock according to a third embodiment of the present disclosure. The cock 62 in FIG. 6 includes a cock main body 40A having a cylindrical shape, a seal member 10A having a cylindrical shape that is slidably and rotatably attached to the cock main body 40A, and connected to the upper side of the cock main body 40A. The first tube body 20 is provided with a first tube body 20, and the second tube body 30 is connected to the lower side of the cock body portion 40A. The seal member 10A has a handle portion 14A on the proximal end side. The seal member 10A is inserted into the cock body 40A from the tip side.

Three ring-shaped sliding parts 18A, 18B, and 18C are attached to the seal member 10A along the circumferential direction. The sliding parts 18A, 18B, and 18C are, for example, resin rings. When the seal member 10A is rotated or slid with respect to the cock body 40A, the sliding parts 18A, 18B, and 18C rotate or slide while sliding against the inner wall surface 42A of the cock body 40A. The sliding parts 18A, 18B, and 18C are attached at predetermined intervals in this order from the distal end to the proximal end of the seal member 10A. The recessed portion 12 is formed within a region defined by the sliding portion 18A and the sliding portion 18B. A gas hole 44 is provided at the tip of the cock body portion 40A that faces the tip of the seal member 10A. By providing the gas hole 44, gas can be circulated between the inside and outside of the cock body 40A.

The first tube 20 is connected to the tip side of the cock body 40A, whereas the second tube 30 is connected to the center of the cock body 40A. That is, when viewed along the sliding direction, the first tubular body 20 and the second tubular body 30 are connected so as to be shifted from each other. When such a cock 62 is used, the sample is moved from the first tube 20 side to the second tube 30 side by the following operation.

As shown in FIG. 6, the sealing member 10A is inserted deep into the cock body 40A. If the gas hole 44 is left open when inserting the seal member 10A, the gas hole 44 functions as a gas vent inside the cock body 40A, and the seal member 10A can be inserted smoothly. Then, the seal member 10A is rotated relative to the cock body 40 using the handle portion 14A, and the seal member 10A is aligned so that the recess 12 formed in the seal member 10A is exposed to the flow path of the first tube body 20. After alignment, a sample is introduced from the flow path of the first tube 20 and accommodated in the recess 12 . At this time, since the flow path of the second tube 30 is located between the sliding portion 18B and the sliding portion 18C, the airtightness of the flow path of the second tube 30 is maintained satisfactorily.

Next, perform an operation to slide the handle portion 14A relative to the cock body portion 40A, and align the connection portion between the cock body portion 40A and the second pipe body 30 between the sliding portions 18A and 18B. I do. This brings the cock 62 into the state shown in FIG. If the gas hole 44 is left open during this operation, the gas hole 44 will function as a gas inlet and the seal member 10A can slide smoothly. In this state, the sample is held in the recess 12.

Subsequently, the handle portion 14A is operated to rotate the sealing member 10A by half a turn relative to the cock body portion 40A, and the recess 12 is rotated downward to bring the cock 62 into the state shown in FIG. The recess 12 rotates as the seal member 10A rotates and is exposed to the flow path of the second tube 30. Also at this time, since the recessed portion 12 is formed within the region defined by the sliding portion 18A and the sliding portion 18B, the airtightness of the flow path of the second tubular body 30 is maintained well. As shown in FIGS. 6 to 8, when the second tube 30 is located lower than the first tube 20, when the state shown in FIG. 8 is reached, it is accommodated in the recess 12 in the state shown in FIGS. The sample, which was being held there, falls downward in the flow path of the second tube body 30 due to gravity. Since the sample can be dropped using gravity in this way, the sample can be introduced into a reactor or the like connected below the second tube 30 with an extremely simple operation.

After dropping the sample from the recess 12 in the state shown in FIG. 8, when the sealing member 10A is further rotated by half a turn with respect to the cock body 40A, the state returns to the state shown in FIG. Then, when the seal member 10A is slid and inserted into the cock body 40A, the state shown in FIG. 6 is restored. At this time, if the gas hole 44 is left open, the seal member 10A can be inserted smoothly. In the state shown in FIG. 6, the sample may be introduced into the recess 12 again via the flow path of the first tube 20. In this way, the recess 12 corresponding to the sample holding section can repeatedly accommodate (hold) and release the sample.

The seal member 10A does not have a through hole that allows the first tube body 20 and the second tube body 30 to communicate with each other. Therefore, it is possible to suppress the flow of a medium such as gas between the first tube 20 and the second tube 30. Further, the seal member 10A has sliding parts 18A, 18B, and 18C that slide on the inner wall surface 42 of the cock body 40A when the seal member 10A slides and rotates, and the flow path of the second pipe body 30 is It is not designed to communicate with the outside world. Therefore, even while the handle portion 14 is being operated, it is possible to sufficiently prevent outside air from entering the second tube body 30 from both ends of the cock body portion 40A.

The cock 62 introduces the sample into the recess 12 in the state shown in FIG. 6, and releases the sample from the recess 12 in the state shown in FIG. Also, while operating the handle portion 14A to change the state shown in FIG. 6 to the state shown in FIG. 8 (including, for example, the state shown in FIG. , are continuously blocked by the sliding parts 18A and 18B. In this way, the cock 62 is excellent not only in airtightness but also in blocking performance between the first tube body 20 and the second tube body 30. Therefore, the cock 62 is particularly useful as a sample supply device for a reaction device that requires high airtightness and high barrier properties.

9 to 10 are diagrams showing a seal member and a cock according to a fourth embodiment of the present disclosure. The cock 64 in FIG. 9 includes a cock main body 40C, a seal member 10C slidably attached to the cock main body 40C, a first tube 20 connected to the upper side of the cock main body 40C, and a cock main body 40C. 40C is provided. The seal member 10C has a handle portion 14C on the proximal end side. The seal member 10C is inserted into the cock body 40C from the tip side. The cock body portion 40C and the seal member 10C may have a cylindrical shape or a prismatic shape such as a square pole.

Three ring-shaped sliding parts 18A, 18B, and 18C are attached to the seal member 10C along its surface. The sliding parts 18A, 18B, and 18C are, for example, resin rings. When the seal member 10C is slid with respect to the cock body 40C, the sliding parts 18A, 18B, 18C rotate or slide while sliding against the inner wall surface 42C of the cock body 40C. The sliding parts 18A, 18B, and 18C are attached at predetermined intervals in this order from the distal end to the proximal end of the seal member 10C.

A through hole 12B is formed in the seal member 10C in a region defined by the sliding portion 18A and the sliding portion 18B. The through hole 12B and the inner wall surface 42C of the cock body 40C constitute a holding section for the sample supplied from the first tube 20.

A gas hole 44 is provided at the tip of the cock body 40C that faces the tip of the seal member 10C. Providing the gas hole 44 allows gas to flow between the inside and outside of the cock body 40C.

The first tube 20 is connected to the tip side of the cock body 40C, while the second tube 30 is connected to the center of the cock body 40C. That is, when viewed along the sliding direction, the first tubular body 20 and the second tubular body 30 are connected so as to be shifted from each other. When such a cock 62 is used, the sample is moved from the first tube 20 side to the second tube 30 side by the following operation.

As shown in FIG. 9, the sealing member 10C is inserted deep into the cock body 40C. If the gas hole 44 is left open when inserting the seal member 10C, the gas hole 44 functions as a gas vent inside the cock body 40C, and the seal member 10C can be inserted smoothly. In the state shown in FIG. 9, the seal member 10C and the cock body portion 40C are aligned so that the through hole 12B formed in the seal member 10C communicates with the flow path of the first tube body 20. Positioning can be performed by sliding the seal member 10C relative to the cock body 40 using the handle 14C. In the state shown in FIG. 9, a sample is introduced from the flow path of the first tube body 20, and is introduced into the through hole 12B and held. At this time, since the flow path of the second tube 30 is located between the sliding portion 18B and the sliding portion 18C, the airtightness of the flow path of the second tube 30 is maintained satisfactorily.

Next, grip the handle portion 14C and slide the seal member 10C relative to the cock body portion 40C to bring it into the state shown in FIG. 10. If the gas hole 44 is left open during this operation, the gas hole 44 will function as a gas inlet and the seal member 10C can slide smoothly. In the state shown in FIG. 10, the through hole 12B communicates with the flow path of the second tube body 30. Also at this time, since the through hole 12B is formed between the sliding portion 18A and the sliding portion 18B, the airtightness of the flow path of the second tube body 30 is maintained well.

As shown in FIGS. 9 and 10, when the second tube 30 is located lower than the first tube 20, when the state shown in FIG. 10 is reached, the state shown in FIG. The sample falls downward in the flow path of the second tube 30 due to gravity. Since the sample can be dropped using gravity in this way, the sample can be introduced into a reactor or the like connected below the second tube 30 with an extremely simple operation.

After dropping the sample from the through hole 12B in the state shown in FIG. 10, if the seal member 10C is slid and inserted into the cock body 40C, the state shown in FIG. 9 is returned. At this time, if the gas hole 44 is left open, the seal member 10C can be inserted smoothly. In the state shown in FIG. 9, the sample may be introduced into the through hole 12B again via the flow path of the first tube body 20. In this way, the seal member 10C and the cock 64 can repeatedly hold and release the sample.

Since the sealing member 10C has the through hole 12B, the sample can be moved from the first tube 20 side to the second tube 30 side by sliding the sealing member 10C with respect to the cock body 40C. Since the through hole 12B does not communicate with both the first tube 20 and the second tube 30 at the same time, it suppresses the flow of a medium such as gas between the first tube 20 and the second tube 30. can. Further, the seal member 10C has sliding portions 18A, 18B, and 18C that slide on the inner wall surface 42 of the cock body portion 40C when the seal member 10C slides, and the flow path of the second pipe body 30 is connected to the outside. They are no longer communicating. Therefore, even while operating the handle portion 14C, it is possible to sufficiently prevent outside air from entering the second tube body 30 from both ends of the cock body portion 40C.

The cock 64 introduces the sample into the through hole 12B in the state shown in FIG. 9, and releases the sample from the through hole 12B in the state shown in FIG. Further, even while operating the handle portion 14C to change the state shown in FIG. 9 to the state shown in FIG. and is blocked. In this way, the cock 62 is excellent not only in airtightness but also in blocking performance between the first tube body 20 and the second tube body 30. Therefore, the cock 64 is particularly useful as a sample supply device for a reaction device that requires high airtightness and high barrier properties.

The seal members 10, 10A, 10B, 10C and cocks 60, 62, 64 according to each of the above embodiments can be used by being connected to various reactors. For example, a reactor used for a reaction that needs to be carried out under an inert gas atmosphere is required to have high airtightness to prevent the inflow of outside air (oxygen). It may also be used by connecting to such a reactor.

The sealing member, cock, and reaction device of the present disclosure can introduce a sample into a reactor with a simple operation while maintaining high sealing performance and airtightness without complicating the device structure. Therefore, work efficiency when handling chemical substances can be improved. Moreover, by performing the process of manufacturing a chemical product using such a reactor, the chemical product can be manufactured efficiently and stably. The chemical product may be a compound, such as an organic compound or an inorganic compound. Further, it may be a final product or an intermediate product.

Although several embodiments have been described above, the present disclosure is not limited to the above embodiments. For example, although the cocks of the above embodiments all had two tube bodies, they may have three or more tube bodies. For example, when three tubes are provided, the first sample may be introduced from the first tube, the first sample may be held in the holding section, and the first sample may be released into the second tube. After that, the second sample may be introduced from the first tube, the second sample may be held in the holding section, and the second sample may be released into the third tube. In this way, the first sample and the second sample, which are different in type from each other, may be configured to be discharged into separate tube bodies.

Further, the reaction device shown in FIG. 4 may have a cock 62 or a cock 64 instead of the cock 60, or may have a seal member 10B shown in FIG. 5. The shutter portion 12A of the seal member 10B, the handle portions 14, 14A of the seal members 10, 10A, and the handle portion 14C of the seal member 10C may be configured to be operated manually, or may be configured to be operated automatically by a control device (not shown). It may be configured to be operated. Further, the shape of the seal member 10 is not particularly limited, and may be, for example, ball-shaped.

The contents of the present invention will be explained in more detail with reference to Examples and Comparative Examples, but the present invention is not limited to the following Examples.
(Example 1)
A glycosylation reaction represented by the following reaction formula (1) was carried out using a reaction apparatus 100 as shown in FIG. 4 equipped with the cock 60 shown in FIGS. 1 and 2. The specific steps were as follows.

The inside of a flask containing a stirrer and molecular sieve 4A (20 mg) was replaced with argon gas. Dichloromethane (0.50 mL), N-iodosuccinimide (68.1 mg, 303 μmol), compound (I) in the above reaction formula (1) (50.6 mg, 84.2 μml), and the alcohol compound in the above reaction formula (1) ( A solution of II) (48.1 mg, 84.3 μmol) was placed in a flask corresponding to reactor 70.

The stopper 86 is opened, and powdered indium triflate (In(OTf) ₃ , 141 mg, 251 μmol) is poured into the recess 12 of the sealing member 10 whose angle is adjusted so that the recess 12 faces upward as shown in FIG. Contained. Thereafter, the stopper 86 was closed, the sealing member 10 was rotated, and indium triflate was dropped into the flask via the second tube 30 and mixed with the solution. Dry ice and ethanol were placed in a temperature control tank 95 to cool the mixture in the flask, and the mixture was allowed to react at -78°C to -40°C for 45 minutes while stirring with a stirrer. Then, at -78°C, a dichloromethane solution (alcohol concentration: 1M) of the alcohol of formula (IV) below (125 μL, 125 μmol) dissolved in dichloromethane was added to the reaction solution, and the temperature was raised to 0°C over 60 minutes with stirring. Then, a saturated aqueous solution of sodium thiosulfate and sodium hydrogencarbonate was added to stop the reaction.

The organic layer was dried using anhydrous sodium sulfate and concentrated under reduced pressure. The concentrated solution was purified using silica gel chromatography (solvent: hexane/ethyl acetate = 10/1 to 5/1) to obtain a colorless product. As a result of analysis of the product, it was confirmed that the reaction represented by the above reaction formula (1) was proceeding. The yield of glucopyranoside (58.7 mg, 54.0 μmol) represented by formula (III) was 64%.

The analysis results of glucopyranoside were as follows.
・Specific luminosity: [α] _D ²¹ +11.15 (c 0.90, CHCl ₃ )
・Refractive index: R _f = 0.43 (hexane/EtOAc = 2/1)
・IR analysis: 2891, 1727, 1271, 1094, 1027, 700 cm ^-1

・^1H NMR (400 MHz, C ₆ D ₆ ): δ 8.18 (dd, J = 7.6, 1.2 Hz, 2H), 8.09 (dd, J = 7.6, 1.2 Hz, 2H), 7.58 (dd, J = 7.6 , 2.0 Hz, 2H), 7.47 (dd, J = 7.6, 2.0 Hz, 2H), 7.30 (d, J = 6.9 Hz, 2H), 7.22 (dd, J = 7.6, 7.6 Hz, 2H), 7.14−6.88 (m, 21H), 6.07 (dd, J = 10.8, 9.6 Hz, 1H), 5.84 (dd, J = 10.8, 7.8 Hz, 1H), 5.34 (d, J = 6.4 Hz, 1H), 5.26 (s, 1H), 5.17 (d, J = 6.4 Hz, 1H), 5.11 (d, J = 6.4 Hz, 1H), 5.06 (d, J = 6.4 Hz, 1H), 4.90 (d, J = 11.9 Hz, 1H) , 4.80−4.67 (m, 3H), 4.59 (d, J = 11.2 Hz, 1H), 4.51 (d, J = 7.8 Hz, 1H), 4.43 (d, J = 11.2 Hz, 1H), 4.36 (d, J = 7.8 Hz, 1H), 4.26 (dd, J = 10.3, 4.8 Hz, 1H), 4.22−4.10 (m, 2H), 4.04 (dd, J = 9.2, 7.8 Hz, 1H), 3.87 (ddd, J = 9.6, 6.0, 6.0 Hz, 1H), 3.81−3.66 (m, J = 7.1 Hz, 2H), 3.66−3.38 (m, 3H), 3.34−3.17 (m, 2H), 2.48 (dd, J = 8.0 , 6.8 Hz, 2H), 1.79-1.55 (m, 2H)

・^13C NMR (100 MHz, C ₆ D ₆ ): δ 166.0, 165.6, 141.9, 138.8, 138.7, 138.2, 138.1, 133.2, 133.1, 130.3, 130.2, 130.1 (2C), 130.0 (2C), 129.1, 128.9 (3C), 128.7 (3C), 128.6 (3C), 128.6 (5C), 128.5 (4C), 127.9 (4C), 127.6, 126.8 (3C), 126.0 (2C), 104.5, 101.8, 101.2, 95.6, 95.4 , 81.4, 77.9, 77.4, 76.8, 75.9, 75.4, 74.9, 72.8, 70.3, 70.0, 69.0, 69.0, 68.7, 66.6, 32.1, 32.4
・High resolution mass spectrometry (HRESIMS): m/z 1109.4303 [M + Na] ⁺ (calcd for C ₆₅ H ₆₆ NaO ₁₅ , 1109.4294)

(Comparative example 1)
Synthesis by glycosylation reaction represented by reaction formula (1) was attempted in the same manner as in Example 1 except that a reaction apparatus without a cock part as shown in FIGS. 1 and 2 was used. In Comparative Example 1, the stopper at the top of the flask was opened and powdered indium triflate was introduced directly into the flask. After the introduction, the stopper was immediately closed, and synthesis was carried out under the same conditions as in Example 1. Analysis of the product obtained by performing a series of operations revealed that the yield of glucopyranoside represented by formula (III) was 1% or less. The reason for such a low yield is thought to be that when indium triflate was introduced, outside air entered and the moisture contained in the outside air inhibited the reaction.

According to the present disclosure, there are provided a seal member, a cock, and a reaction device that can improve work efficiency when handling chemical substances. Further, a method for manufacturing a chemical product that can efficiently manufacture a chemical product is provided.

10, 10A, 10B, 10C... Seal member, 12... Recessed part (holding part), 12A... Shutter part (holding part), 14, 14A... Handle part, 14C... Handle part, 16... Fixing part, 17... Lever, 18 , 18A, 18B, 18C...Sliding part, 20, 30...Pipe body, 40, 40A, 40C...Cook body part, 42, 42A, 42C...Inner wall surface, 44...Gas hole, 50...Packing, 52...Fixing member , 60, 62, 64...cock, 70...reactor, 71...main pipe, 72...side pipe, 74...valve, 76...cap, 82...manifold, 84...needle, 86...stopper, 90...refrigerant, 95... Temperature control tank, 100... Reactor, 110... Raw material liquid.

Claims (6)

comprising at least two pipe bodies including a first pipe body and a second pipe body, a cock main body part connecting these, and a sealing member rotatably attached to the cock main body part ,
The sealing member has a sliding portion that slides against the inner wall surface of the cock body, and a holding portion that is a recessed portion that holds the sample,
The recessed portion is formed so as to be surrounded by the sliding portion,
The cock is configured such that the concave portion can rotate to move the sample from the first tube side to the second tube side . the second tube is located lower than the first tube;
The cock according to claim 1, wherein when the recess rotates and is exposed to the flow path of the second tube, the sample accommodated in the recess falls through the flow path due to gravity. The cock according to claim 1 or 2 , wherein the sealing member is slidably attached to a cock body that connects at least two pipes including the first pipe and the second pipe. comprising at least two tubes including a first tube and a second tube , a cock body that connects them, and a seal member that is slidably attached to the cock body ;
The first tube body and the second tube body are connected to the cock body portion so as to be offset from each other when viewed along the sliding direction of the sealing member relative to the cock body portion,
The through hole penetrating the sealing member and the inner wall surface of the cock body constitute a holding part that holds the sample,
The through hole communicates with the flow path of the first pipe body at a first position, and the through hole communicates with the flow path of the first pipe body at a second position where the seal member is slid with respect to the cock body from the first position. communicates with the flow path of the pipe body,
A cock configured to be able to move the sample from the first tube side to the second tube side without communicating the first tube body and the second tube body. comprising the cock and reactor according to any one of claims 1 to 4,
The first pipe body is arranged above the cock body, and the second pipe body is arranged below the cock body, and the second pipe body and the reactor are connected. ,
A reaction device in which the sample introduced from the first tube and accommodated in the holding section falls from the holding section into the reactor via the second tube by operating the cock . A method for manufacturing a chemical product, comprising the step of manufacturing the chemical product using the reaction apparatus according to claim 5 .

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