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Preparation method of methyl 3-cyano-4-hydroxybenzoate

A technology of methyl hydroxybenzoate and cyano, which is applied in the field of preparation of methyl 3-cyano-4-hydroxybenzoate, can solve problems such as serious hazards, and is suitable for mass production, with obvious cost advantages and cheap raw materials Easy to get effect

Inactive Publication Date: 2017-05-17
SUZHOU BLUEHILL BIOPHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The biggest defect of this process is that cuprous cyanide, a highly toxic cyanide, is used in the process, which is relatively harmful in the actual market.

Method used

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  • Preparation method of methyl 3-cyano-4-hydroxybenzoate
  • Preparation method of methyl 3-cyano-4-hydroxybenzoate
  • Preparation method of methyl 3-cyano-4-hydroxybenzoate

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Embodiment

[0015] 1) Add methyl 4-hydroxybenzoate (2.5kg, 16.4mol), magnesium chloride (3.2kg, 32.8mol), triethylamine (9.3L, 82mol), paraformaldehyde (3.9kg, 131.2 mol), dichloromethane (18L), heated in an oil bath at 60°C (internal temperature 44°C) overnight. After cooling to room temperature, slowly add 5 L of concentrated hydrochloric acid diluted aqueous solution, filter off the insoluble matter, extract with DCM 4 times, dry over sodium sulfate, filter and spin dry. directly to the next step.

[0016] 2) Add the raw materials of the previous step into the 50L reaction pot, hydroxylamine hydrochloride (1.14kg) and acetonitrile / N,N-dimethylformamide (10L / 2.5L), add acetyl chloride (1.17L), heat and stir at 80°C for 2 hours . After cooling to room temperature, add 10L of EA, wash with 5L of water twice, reverse extraction with water once, combine the organic layers, dry over sodium sulfate, filter, spin until half dry, a large amount of solid precipitates, directly suction filter, ...

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Abstract

The invention discloses a preparation method of methyl 3-cyano-4-hydroxybenzoate. The method comprises the steps of 1, preparing methyl 3-hydroxybenzoate into methyl 3-formyl-4-hydroxybenzoate; 2, preparing the methyl 3-formyl-4-hydroxybenzoate into the methyl 3-cyano-4-hydroxybenzoate. The preparation method of the methyl 3-cyano-4-hydroxybenzoate has the advantages that (1) highly toxic cyanide, i.e., cuprous cyanide used in the previous process is avoided being used in the preparation method, so that the preparation method is more suitable for industrialization; (2) a cyano group is prepared from a formyl group, so that the method is efficient and direct and is suitable for mass production; (3) the raw material is cheap and easy to obtain, so that the method is obvious in cost advantage.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a preparation method of methyl 3-cyano-4-hydroxybenzoate. Background technique [0002] The traditional process for preparing methyl 3-cyano-4-hydroxybenzoate is as follows: [0003] [0004] The relatively big defect that this process exists is that the cuprous cyanide of highly toxic cyanide has been adopted in the process of the process, which has relatively large harm in the actual market. Contents of the invention [0005] The object of the present invention is to provide a kind of preparation method of 3-cyano group-4-hydroxybenzoic acid methyl ester, aims to solve the above problems. [0006] In order to achieve the above object, technical scheme of the present invention is to design a kind of preparation method of 3-cyano-4-hydroxybenzoic acid methyl ester, comprises the steps: [0007] 1) Add magnesium chloride, triethylamine, paraformaldehyde, and dichl...

Claims

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Application Information

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IPC IPC(8): C07C255/57C07C253/00
CPCC07C67/313C07C253/00C07C255/57C07C69/76
Inventor 池永贵黄轩
Owner SUZHOU BLUEHILL BIOPHARMA CO LTD
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