JPS6197028A - Reaction vessel - Google Patents

Abstract

PURPOSE:To reduce the fitting misses between a branch pipe for an opening port and a tube by providing plural branch pipes for an opening port fitted with a tube for supplying a raw material, discharging a product, etc., and arranging the junction port pats of said branch pipes in parallel with each other. CONSTITUTION:When an intermediate product <11>CH3OH of <11>CH3I is synthesized, for example, a supporting part 23 for supporting a reaction vessel 10 and a reaction furnace 22 are provided to a synthesis apparatus fitted with the reaction vessel 10. A heater 4 and a nozzle 25 for spouting liquiefied CO2 (at about-20 deg.C) for cooling are furnished to the reaction furnace 22. A flexible tube made of 'Teflon(R)' is used as tubes 26, 27, and 28 to be fitted into branch pipes 15, 16, and 17 of the reaction vessel 10, and supported by fittings 29-1, 29-2, and 29-3 at positions corresponding to the branch pipes 15, 16, and 17. The tube 26 is used for evacuation, the tube 27 is used for discharging the product <11>CH3OH, and the tube 28 is used for supplying the raw gaseous <11>CO2.

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a reaction vessel used in an automatic synthesizer for synthesizing compounds such as labeled compounds.

(Prior Art) A reaction vessel of an automatic synthesis apparatus requires a plurality of openings for supplying raw materials, taking out products, or venting air.

For example, Fig. 3 shows a glass reduction reaction vessel 1 used when synthesizing the labeled compound "CH31."The lower part of this reaction vessel is equipped with a branch pipe for opening because it is housed in an electric furnace. There are five branch pipes with the same diameter at the top.
6 is provided. Branch pipe 2 is for supplying a solution in which the reducing agent LiAfiH4 is dissolved in the solvent tetrahydrofuran (hereinafter referred to as THE), and the branch pipe 3 is for supplying the intermediate product.
The branch pipe 4 is for vaporizing and taking out CH30H, the branch pipe 5 is for evacuation, the branch pipe 5 is for supplying raw material gas '1cO2, and the branch pipe 6 is for supplying water. The branch pipes 2 to 4 are connected directly to the lower space 7, and the branch pipes 5 and 6 are connected to the lower space 7 via an internal pipe 8 led to the bottom of the lower space 7.

When this reaction vessel 1 is used, flexible tubes made of Teflon (registered trademark of DuPont) are attached to each branch pipe 2 to 6 by joints, and raw materials are supplied and products are taken out through these tubes. will be carried out.

(Problems to be Solved by the Invention) In automatic synthesizers for labeled compounds, the reaction vessels are frequently replaced after each synthesis, even in Koe and other automatic synthesizers.
Each time, the branch pipes 2 to 6 and the joint of each tube must be attached and detached.

However, in the reaction vessel 1 shown in FIG. 3, the connection ports of the branch pipes 2 to 6 are oriented in all directions, so the tubes attached to them are also oriented in all directions. It gets longer. Therefore, when the joint is once removed from the branch pipes 2 to 6 and then reattached, there is a risk that the joint will be placed in the wrong position, partly because the diameters of the branch pipes 2 to 6 are the same. In addition, the tubes become entangled in the air, and the reaction vessel 1
There is also the risk of getting caught and causing an accident. Misfitting and accidents between branch pipes 2 to 6 and the tubes are unforgivable in any automatic synthesis equipment, but especially in equipment that handles radioactive isotopes, such as automatic synthesis equipment for S-brittle compounds. Mistakes and accidents like this should never happen.

SUMMARY OF THE INVENTION An object of the present invention is to provide a reaction container in which mistakes in fitting the opening branch pipe and tube of one reaction container and entanglement of the tubes do not occur.

(Means for Solving the Problems) The reaction vessel of the present invention has connecting ports of a plurality of branch pipes to which tubes for supplying raw materials, taking out products, etc. are installed parallel to each other. be.

(Function) Since the connection ports of the branch pipes to which the tubes are attached are made parallel to each other, if the joints or tubes are supported while maintaining the relative positional relationship between the tubes attached to each branch pipe, Since the correspondence between the branch pipe and the tube is maintained, the tube is always attached to the correct branch pipe when the branch pipe and the tube are attached or detached.

In addition, the tubes can be arranged in an orderly manner in accordance with the arrangement of the branch pipe connection ports. (Example) FIG. 1 is a cross-sectional view of a glass reaction vessel 10 according to an example. It is. Inside, a lower space 1 is created by a partition wall 11.
2 and an upper space 13, and the lower space 12 is housed in the reactor when the reaction vessel 10 is installed in the reactor. The lower space 12 and the upper space 13 are connected by an internal pipe 14, and the opening at the tip of the internal pipe 14 is located at the bottom of the lower space 12.

Five opening branch pipes 15 to 19 are provided above the partition wall 11. The branch pipes 15 and 16 lead to a common internal pipe 20 provided in the upper space 13 and which has an opening into the lower space 12. Branch pipe 17 has an opening in upper space 13 .

These branch pipes 15 to 17 are for attaching tubes by joints, and each connection port part,
That is, the external opening portions are provided so as to be parallel to each other in a plane.

The branch pipe 18 passes through the upper space 13 and has an opening into the lower space 12 , and the branch pipe 19 has an opening into the upper space 13 . These branch pipes 18 and 19 are for reagent injection, and a septum is fitted into the external opening, and the reagent is injected with a syringe through the septum.

Next, the cost of using the reaction vessel 10 of this example will be explained using FIG. 2 as an example for synthesizing the labeled compound "CH30H," which is an intermediate product of CH3I.

One reaction vessel 10 is installed in the synthesis apparatus to which the reaction vessel 10 is attached.
A support member 23 and a reactor 22 are provided, and the reactor 22 includes a heater 24 and a cooling liquefied CO2 (about -
A nozzle 25 is provided which ejects a temperature (set at 20°C). As the support member 23, a spring-type clamp or the like is suitable.As the tubes 26-28 attached to the branch pipes 15-17 of the reaction vessel 10, flexible tubes made of Teflon are used. - 17 are supported by metal fittings 29-1 to 29-3 provided on the support plate 29, and Teflon joints 30 to 32 are attached to the tips of each tube 26 to 28. Tube 26 is for vacuum evacuation, tube 27 is for product "CHaO"
The tube 28 is for extracting the raw material gas I1. C
This is for O2 supply.

The reaction vessel 10 is supported by a support member 23 so that its lower space 12 is accommodated within the reaction furnace 22 .

Next, each of the branch pipes 15 to 17 is connected to a corresponding tube 2.
The branch pipes 15 to 17 are inserted into the joints 30 to 32 of 6 to 28, and the screws of the joints 30 to 32 are tightened to connect the branch pipes 15 to 17 and the joints 30 to 32. A septum 33, 34 is fitted into the external opening of the branch pipe 18, 19 to seal it.

“The order of CH308 synthesis is as follows.

(1) While cooling the lower space 12 of the reaction vessel 10 to about -20°C by spouting liquefied CO2 from the nozzle 25 of the reactor 22, a solution of LiAΩH4 dissolved in THF is injected into the branch pipe 18 using a syringe. is injected through the septum 33 into the lower space 12 of the reaction vessel 10.

(2) While cooling the reaction vessel 10 to about -20°C,
1 lcO2 gas is sent from the tube 28 through the branch pipe 17 and blown into the L i A QH4 solution from the tip of the internal pipe 14 to reduce GO2.

(3) The heater 24 of the reaction furnace 22 is energized and the reaction vessel 10
The lower space of the branch pipe 15 is heated to approximately 100°C.
Then, vacuum evacuation is performed through the tube 26 to evaporate THF, which is a solvent.

(4) The reaction vessel 22 lowers the reaction vessel lower space 12 by approximately -2
While cooling to 0°C, water is injected through the septum 34 of the branch 19 using a syringe. This is J,”CH30H
is generated.

(5) Heating is performed in the reactor 22 to vaporize CH30H and take it out from the branch pipe 16 through the tube 27.

In order to generate CH3I from CH30H, a similar apparatus may be used to react C:HsOH with HI.

Although the example shows three branch pipes to which tubes are attached, the number of branch pipes is not limited to this.
In short, if there are a plurality of branch pipes to which tubes are attached, it is sufficient that their connection ports are parallel to each other, and the internal structure of the reaction vessel is not limited to that of the example. do not have.

(Effects of the Invention) According to the reaction container of the present invention, since the connection port portions of the branch pipes for opening are parallel to each other, the tubes can be attached and detached while maintaining the correspondence between the branch pipes and the tubes attached thereto. This eliminates tube attachment errors when replacing one reaction container.

Furthermore, since the tubes can be arranged in an orderly manner in accordance with the arrangement of the branch pipe connection ports, the tubes will not become entangled in the air.

[Brief explanation of drawings]

Fig. 1 is a sectional view showing an embodiment of the present invention, Fig. 2 is a schematic sectional view showing an example of the use of the same embodiment, and Fig. 3 is a front sectional view showing a conventional reaction vessel. ...Reaction container, 15.16,17... Branch pipe to which the tube is attached. 26.27,28...Tube.

Claims (2)

[Claims] (1) A reaction vessel that is equipped with a plurality of opening branch pipes to which tubes for supplying raw materials, taking out products, etc. are attached, and in which the connection ports of these branch pipes are provided in parallel to each other. (2) The reaction container according to claim 1, wherein the tubes attached to the branch pipes are arranged parallel to each other in accordance with the arrangement of the branch pipe connection ports, and are supported by support means.