Method for preparing phenylthioacetate

A phenylacetic acid and thiol technology, applied in sulfide preparation, organic chemistry and other directions, can solve the problems of difficulty in improving the purity of disposable products, many changes in impurities in the finished product, and high cost of secondary refining, so as to reduce the risk of reaction and reduce production. cost, the effect of reducing the pollution of the three wastes

Inactive Publication Date: 2014-09-10
JINTAN DEPEI CHEM
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Problems solved by technology

[0014] The product yield is only 25% to 28%, and there are many impurities in the finished product, the color is unstable, and the product purity is only 90% to 92%. It is difficult to improve the purity of disposable products, the cost of secondary refining is high, and the pollution of three wastes is large

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  • Method for preparing phenylthioacetate

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Embodiment 1

[0028] The present invention uses o-chlorobenzaldehyde and p-chlorothiophenol as raw materials to carry out the condensation reaction with o-chlorobenzaldehyde and p-chlorothiophenol as raw materials under the condition that toluene is used as a solvent, and then reacts with hippuric acid in acetic anhydride , a cyclization reaction occurs in the presence of sodium acetate, and finally hydrolyzed and oxidized to finally obtain the product thiophenylacetic acid; the specific steps are as follows:

[0029] Step 1, condensation reaction: In a 1000ml four-neck flask, put 500ml of toluene, 200g of o-chlorobenzaldehyde, 190g of p-chlorothiophenol, 10g of anhydrous potassium carbonate, heat up to 50-60°C, react for 3-4 hours, cool to below 5°C, filtered, washed with water to obtain thiobenzaldehyde, and dried to obtain 349 g of dry thiobenzaldehyde, with a yield of 98.5%.

[0030] Step 2, ring closure reaction: In a 2000ml four-necked flask, put 1000g of acetic anhydride, 349g of thi...

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Abstract

The invention discloses a method for preparing phenylthioacetate. According to the method, o-chlorobenzaldehyde and p-chlorothiophenol raw materials are reacted in methylbenzene at a low temperature, so that o-chloroacetophenone serving as a raw material is abandoned; the o-chlorobenzaldehyde substitutes the o-chloroacetophenone, the methylbenzene is used as a solvent, and the condensation reaction can be performed at 50-60 DEG C, so that high-temperature condensation is not needed, the reaction is mild, the reaction hazard is reduced, three-waste pollution is reduced, the reaction yield is increased, and the cost is reduced. Hippuric acid substitutes morpholine, and the methylbenzene substitutes dioxane, so that the production cost is greatly reduced, and the reaction yield is increased. The yield of the product reaches 94%, the purity of the one-off product is more than 99%, secondary refining is not needed, and the color stability is good.

Description

Technical field: [0001] The invention relates to a preparation method of thiophenylacetic acid. Background technique: [0002] The chemical name of thiophenylacetic acid: 2-p-chlorophenylthiophenylacetic acid, CAS registration number: 13459-62-6 [0003] Thiophenylacetic acid is the key raw material for the production of zotepine, which is a methepine antipsychotic drug. [0004] The research on the synthesis of thiophenylacetic acid has been continuously improved and improved. At present, the mainstream production methods of thiophenylacetic acid are as follows: [0005] ①Using o-chloroacetophenone as raw material: [0006] It uses o-chloroacetophenone as the raw material, first undergoes a coupling reaction with p-chlorothiophenol, then undergoes a condensation reaction with morpholine, and then undergoes hydrolysis to generate thiophenylacetic acid. [0007] The synthesis process is as follows: o-chloroacetophenone and p-chlorothiophenol, under the catalysis of cuprous...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/62C07C319/20
Inventor 叶荫胡汉志叶锡培冯俊戴起福
Owner JINTAN DEPEI CHEM
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