CN217431663U

CN217431663U - Grignard reaction device for preparing sartanbiphenyl

Info

Publication number: CN217431663U
Application number: CN202221075692.2U
Authority: CN
Inventors: 陈诚乐; 吴丙华
Original assignee: Jiangxi Dadi Pharm Co ltd
Current assignee: Jiangxi Dadi Pharm Co ltd
Priority date: 2022-05-07
Filing date: 2022-05-07
Publication date: 2022-09-16
Anticipated expiration: 2032-05-07

Abstract

The utility model discloses a grignard reaction device for preparing sartanbiphenyl, including settling cask, retort and condenser, the nitrogen gas mouth has been seted up to the upper surface of settling cask, upper surface one side fixed mounting of settling cask has the evacuation pipe, the upper surface opposite side fixed mounting of settling cask has grignard liquid to change the material pipe, the upper surface demountable installation of retort has the cover, the lower surface movable mounting of cover has the stirring post, upper surface one side fixed mounting of cover has active magnesium powder to change the material pipe, upper surface one side fixed mounting of cover has the inlet pipe, the upper surface of cover, the one side fixed mounting who is located the inlet pipe have the nitrogen gas pipe. The utility model has the advantages that the content of p-tolyl magnesium chloride in the Grignard solution is more than 99.0 percent; the yield of sartanbiphenyl (2-cyano-4-methyl biphenyl) is 88-90%, the content is more than 99.0%, the yield is improved than 85% reported in the literature, and the sartanbiphenyl (2-cyano-4-methyl biphenyl) has practicability.

Description

Grignard reaction device for preparing sartanbiphenyl

Technical Field

The utility model relates to the field of equipment for drug synthesis, in particular to a Grignard reaction device for preparing sartanbiphenyl.

Background

Sartanbiphenyl (2-cyano-4-methylbiphenyl) is a basic intermediate for synthesizing medicaments for treating cardiovascular diseases, such as irbesartan, candesartan, telmisartan, tasosartan and the like, has an antihypertensive effect and a certain curative effect on cardiac insufficiency, and belongs to an angiotensin II receptor anticaking agent. They have stable pressure reduction, less side reaction and long-acting property. At present, the main method for industrially producing sartanbiphenyl is to prepare sartanbiphenyl by taking p-chlorotoluene as a raw material and carrying out Grignard reaction on the raw material to prepare a p-methyl magnesium chloride Grignard reagent, and then reacting the p-methyl magnesium chloride Grignard reagent with o-chlorobenzonitrile. The Grignard reaction is an anhydrous and anaerobic reaction, an initiator is added to carry out the reaction, and moisture and air are prevented from entering a reaction system during the reaction process and sampling monitoring; in addition, the prepared Grignard reaction solution also contains a part of excessive active magnesium powder, and side reaction can occur during the condensation reaction of the Grignard reaction solution and the o-chlorobenzonitrile, thereby influencing the purity and the yield of the product.

SUMMERY OF THE UTILITY MODEL

The utility model aims to provide a grignard reaction device for preparing sartanbiphenyl, which can effectively solve the problems in the background technology.

In order to achieve the above purpose, the utility model adopts the following technical scheme:

the utility model provides a grignard reaction device for preparing sartanbiphenyl, includes settling cask, retort and condenser, the nitrogen gas mouth has been seted up to the upper surface of settling cask, upper surface one side fixed mounting of settling cask has the evacuation pipe, the upper surface opposite side fixed mounting of settling cask has grignard liquid to change the material pipe, the upper surface demountable installation of retort has the cover, the lower surface movable mounting of cover has the stirring post, upper surface one side fixed mounting of cover has active magnesium powder to change the material pipe, upper surface one side fixed mounting of cover has the inlet pipe, the upper surface of cover, the one side fixed mounting who is located the inlet pipe have a nitrogen gas pipe, the dropwise add mouth has been seted up to the upper surface of cover.

Preferably, the upper surface of the tank cover is detachably provided with a return pipe, and the return pipe is detachably connected with the condenser.

Preferably, the upper end of the tank cover is fixedly provided with a motor, and the stirring column is fixedly connected with the output end of the motor.

Preferably, a pipe joint is fixedly mounted on the outer surface of the Grignard liquid transfer pipe, a sampling protection pipe is fixedly mounted at one end of the pipe joint, and a sampling port is formed below the outer surface of the sampling protection pipe.

Preferably, all fixed mounting has the stand around the lower surface of settling cask, the other end and the cover fixed connection of grignard liquid material transfer pipe.

Preferably, the lower surface of the settling tank and the reaction tank is fixedly provided with a discharging pipe, one end of the active magnesium powder transferring pipe is fixedly connected with the discharging pipe on the settling tank, and a clear liquid dripping pipe is fixedly arranged at the joint of one end of the active magnesium powder transferring pipe and the discharging pipe of the settling tank.

Compared with the prior art, the utility model discloses following beneficial effect has:

1. the utility model has the advantages that the content of p-tolyl magnesium chloride in the Grignard solution is more than 99.0 percent; the yield of sartanbiphenyl (2-cyano-4-methyl biphenyl) is 88-90%, the content is more than 99.0%, and the yield is improved compared with 85% reported in the literature; meanwhile, excessive active metal magnesium in the Grignard solution is settled and then sits down with a batch of reaction initiator, so that the cost is saved and the method has practicability.

Drawings

FIG. 1 is a schematic diagram of the overall structure of a Grignard reaction apparatus for preparing sartanbiphenyl according to the present invention;

fig. 2 is a schematic structural diagram of a reaction tank in a grignard reaction apparatus for preparing sartanbiphenyl of the present invention.

In the figure: 1. a feed pipe; 2. a nitrogen gas pipe; 3. a dropping port; 4. a return pipe; 5. a Grignard liquid transfer pipe; 6. an active magnesium powder transferring pipe; 7. a clear liquid dropping pipe; 8. a sampling protection tube; 9. A nitrogen port; 10. emptying the pipe; 11. a sampling port; 12. a settling tank; 13. a column; 14. a reaction tank; 15. a condenser; 16. a can lid; 17. a motor; 18. the column was stirred.

Detailed Description

In order to make the technical means, creation features, achievement purposes and functions of the present invention easy to understand, the present invention is further described below with reference to the following embodiments.

In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front end", "rear end", "both ends", "one end", "the other end" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the device or element to which the reference is made must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.

In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "connected," and the like are to be construed broadly, and for example, "connected" may be either fixedly connected or detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art.

As shown in fig. 1-2, a grignard reaction device for preparing sartanbiphenyl, which comprises a settling tank 12, a reaction tank 14 and a condenser 15, wherein a nitrogen port 9 is formed in the upper surface of the settling tank 12, an emptying pipe 10 is fixedly mounted on one side of the upper surface of the settling tank 12, a grignard liquid transfer pipe 5 is fixedly mounted on the other side of the upper surface of the settling tank 12, a tank cover 16 is detachably mounted on the upper surface of the reaction tank 14, a stirring column 18 is movably mounted on the lower surface of the tank cover 16, an active magnesium powder transfer pipe 6 is fixedly mounted on one side of the upper surface of the tank cover 16, an inlet pipe 1 is fixedly mounted on one side of the upper surface of the tank cover 16, the upper surface of the tank cover 16 and one side of the inlet pipe 1 are fixedly mounted with a nitrogen pipe 2, and a dropping port 3 is formed in the upper surface of the tank cover 16.

The return pipe 4 is detachably mounted on the upper surface of the tank cover 16, the return pipe 4 is detachably connected with the condenser 15, and the liquid conveyed to the condenser 15 and condensed can be returned to the reaction tank 14 through the return pipe 4.

The upper end of the tank cover 16 is fixedly provided with a motor 17, the stirring column 18 is fixedly connected with the output end of the motor 17, and the motor 17 on the tank cover 16 can drive the stirring column 18 to start stirring, so that mixing is performed.

The outer surface of the Grignard liquid transfer pipe 5 is fixedly provided with a pipe joint, one end of the pipe joint is fixedly provided with a sampling protection pipe 8, and a sampling port 11 is arranged below the outer surface of the sampling protection pipe 8.

All fixed mounting has stand 13 around the lower surface of settling cask 12, and the other end and the cover 16 fixed connection of grignard liquid material transfer pipe 5, stand 13 are used for supporting settling cask 12.

The equal fixed mounting of lower surface of settling cask 12 and retort 14 has the discharging pipe, and the active magnesium powder changes discharging pipe fixed connection on one end of material pipe 6 and the settling cask 12, and the active magnesium powder changes the one end of material pipe 6, is located and has clear liquid dropwise add pipe 7 with the junction fixed mounting of settling cask 12 discharging pipe, can change dropwise add medicament in the material pipe 6 to active magnesium powder through clear liquid dropwise add pipe 7.

It should be noted that, the utility model relates to a grignard reaction device for preparing sartanbiphenyl, firstly, the nitrogen pipe 2 is used to replace the air in the dry reaction tank 14 for three times, then the metal magnesium chips are put into under the protection of nitrogen, the solvent and the initiating agent are added from the feeding pipe 1, the motor 17 on the tank cover 16 can drive the stirring column 18 to start stirring; dripping a medicament into the p-chlorotoluene to react; after the reaction is finished, closing the evacuation of a reaction system, adding 0.01-0.1 MPa of nitrogen pressure, sampling and detecting from a self-designed sampling port 11, taking a sample, pressurizing the sample from a nitrogen port 9, taking the sample from a sampling pipeline, pressing the sample back to a reaction tank 14, stopping stirring after the reaction is qualified, after settling for 1-2 hours, transferring the supernatant to a high-level settling tank 12 through a Grignard liquid transfer pipe 5, settling for 4-10 hours, the bottom of the settled material liquid contains magnesium powder, then transferring to the reaction tank 14, wherein the initiator is used for the reaction of the next batch of materials, a stand 13 plays a supporting role, the condensation reaction of the supernatant and o-chlorobenzonitrile, and a reaction result: the content of p-tolyl magnesium chloride was 99.2%, the yield of sartanbiphenyl (2-cyano-4-methylbiphenyl) was 89%, and the content was 99.0%.

The basic principles and the main features of the invention and the advantages of the invention have been shown and described above. It will be understood by those skilled in the art that the present invention is not limited to the above embodiments, and that the foregoing embodiments and descriptions are provided only to illustrate the principles of the present invention without departing from the spirit and scope of the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims

1. The utility model provides a Grignard reaction device for preparing sartanbiphenyl, includes settling cask (12), retort (14) and condenser (15), its characterized in that, nitrogen gas mouth (9) have been seted up to the upper surface of settling cask (12), upper surface one side fixed mounting of settling cask (12) has evacuation pipe (10), the upper surface opposite side fixed mounting of settling cask (12) has Grignard liquid to change material pipe (5), the upper surface demountable installation of retort (14) has cover (16), the lower surface movable mounting of cover (16) has stirring column (18), the upper surface one side fixed mounting of cover (16) has active magnesium powder to change material pipe (6), the upper surface one side fixed mounting of cover (16) has inlet pipe (1), the upper surface of cover (16), the one side fixed mounting that is located inlet pipe (1) have nitrogen gas pipe (2), the upper surface of the tank cover (16) is provided with a dropping port (3).

2. The Grignard reaction device for preparing sartanbiphenyl according to claim 1, wherein a return pipe (4) is detachably mounted on the upper surface of the tank cover (16), and the return pipe (4) is detachably connected with the condenser (15).

3. The Grignard reaction device for preparing sartanbiphenyl according to claim 1, wherein a motor (17) is fixedly installed at the upper end of the tank cover (16), and the stirring column (18) is fixedly connected with the output end of the motor (17).

4. The Grignard reaction device for preparing sartanbiphenyl according to claim 1, wherein a pipe joint is fixedly installed on the outer surface of the Grignard liquid transfer pipe (5), a sampling protection pipe (8) is fixedly installed at one end of the pipe joint, and a sampling port (11) is formed below the outer surface of the sampling protection pipe (8).

5. The Grignard reaction device for preparing sartanbiphenyl according to claim 1, wherein the periphery of the lower surface of the settling tank (12) is fixedly provided with the upright posts (13), and the other end of the Grignard liquid transfer pipe (5) is fixedly connected with the tank cover (16).

6. The Grignard reaction device for preparing sartanbiphenyl according to claim 1, wherein discharge pipes are fixedly mounted on the lower surfaces of the settling tank (12) and the reaction tank (14), one end of the active magnesium powder transferring pipe (6) is fixedly connected with the discharge pipe on the settling tank (12), and a clear liquid dropping pipe (7) is fixedly mounted at the joint of one end of the active magnesium powder transferring pipe (6) and the discharge pipe of the settling tank (12).