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Preparation method of 3-cyano-4-isopropoxybenzoic acid

A technology of isopropoxybenzoic acid and phenyl isopropoxybenzoate, which is applied in the field of preparation of 3-cyano-4-isopropoxybenzoic acid, can solve problems such as high hazard, and is suitable for a large number of Production, cost advantages are obvious, and raw materials are cheap and easy to obtain.

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 3-cyano-4-isopropoxybenzoic acid
  • Preparation method of 3-cyano-4-isopropoxybenzoic acid
  • Preparation method of 3-cyano-4-isopropoxybenzoic acid

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Embodiment

[0019] 1) Add 4-hydroxybenzoic acid phenyl ester (3.5kg, 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 suctio...

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Abstract

The invention discloses a preparation method of 3-cyano-4-isopropoxybenzoic acid. The preparation method comprises the following steps: step one, preparing 3-formyl-4-phenyl hydroxybenzoate from 4-phenyl hydroxybenzoate; step two, preparing 3-cyano-4-phenyl hydroxybenzoate from the 3-formyl-4-phenyl hydroxybenzoate; step three, preparing 3-cyano-4-phenyl isopropoxybenzoate from the 3-cyano-4-phenyl hydroxybenzoate; step four, preparing the 3-cyano-4-isopropoxybenzoic acid from the 3-cyano-4-phenyl isopropoxybenzoate. The preparation method of the 3-cyano-4-isopropoxybenzoic acid, disclosed by the invention, has the advantages that (1) the use of a highly toxic cyanide-cuprous cyanide in the prior art is avoided, and the preparation method is more suitable for industrialization; (2) cyanogroup is prepared from formyl groups, and the preparation method is efficient and direct and is suitable for large-scale production; (3) all raw materials are cheap and easy to obtain, and the cost advantage is obvious.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a preparation method of 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 preparation method of 3-cyano group-4-isopropoxybenzoic acid, 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-isopropoxybenzoic acid, comprising the steps: [0007] 1) Add magnesium chloride, triethylamine, paraformaldehyde, and dichloromethane to 4-hyd...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/57
CPCC07C67/343C07C253/00C07C253/30C07C255/57C07C69/94
Inventor 池永贵黄轩
Owner SUZHOU BLUEHILL BIOPHARMA CO LTD
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