Method for preparing 3-cyano-4-isopropoxybenzoic acid

A technology of isopropoxybenzoic acid and methyl hydroxybenzoate, which is applied in the field of preparing 3-cyano-4-isopropoxybenzoic acid, can solve the problems of great harm, and is suitable for mass production and cheap raw materials Easy to obtain and obvious cost advantages

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

Method used

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  • Method for preparing 3-cyano-4-isopropoxybenzoic acid
  • Method for preparing 3-cyano-4-isopropoxybenzoic acid
  • Method for preparing 3-cyano-4-isopropoxybenzoic acid

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Experimental program
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Embodiment

[0019] 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.

[0020] 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 method for preparing 3-cyano-4-isopropoxybenzoic acid. A first step, 3-formyl-4-methyl hydroxybenzoate is prepared with methyl parahydroxybenzoate; a second step, 3-cyano-4-methyl hydroxybenzoate is prepared with the 3-formyl-4-methyl hydroxybenzoate; a third step, 3-cyano-4-methyl isopropoxybenzoate is prepared with the 3-cyano-4-methyl hydroxybenzoate; a fourth step, the 3-cyano-4-isopropoxybenzoic acid is prepared with the 3-cyano-4-methyl isopropoxybenzoate. The preparation method of the 3-cyano-4-isopropoxybenzoic acid, which is provided by the invention, has the advantages that 1) the use of the cuprous cyanide of hypertoxic cyanide in a previous process is avoided, and the method is more suitable for industrialization; 2) cyano is prepared by formyl, and the method is high-efficiency and direct, and is suitable for quantity production; 3) all raw materials are cheap and easily obtained, and the cost advantage is obvious.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a method for preparing 3-cyano-4-isopropoxybenzoic acid. Background technique [0002] The traditional process for preparing 3-cyano-4-isopropoxybenzoic acid 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 method for preparing 3-cyano group-4-isopropoxybenzoic acid, aims to solve the above problems. [0006] In order to achieve the above object, the technical scheme of the present invention is to design a method for preparing 3-cyano-4-isopropoxybenzoic acid, comprising the steps of: [0007] 1) Add magnesium chloride, triethylamine, paraformaldehyde, and dichloromethane to methyl p-...

Claims

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Application Information

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IPC IPC(8): C07C253/30C07C255/57
CPCC07C67/343C07C253/00C07C253/30C07C255/57C07C69/84
Inventor 池永贵黄轩
Owner SUZHOU BLUEHILL BIOPHARMA CO LTD
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