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Preparation method of 3-cyano-4-isopropoxy methyl benzoate

A technology of methyl isopropoxybenzoate and methyl hydroxybenzoate, applied in the field of preparation of methyl 3-cyano-4-isopropoxybenzoate, can solve problems such as high hazard, and achieve suitable Mass production, cheap and easy-to-obtain raw materials, 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

AI Technical Summary

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-isopropoxy methyl benzoate
  • Preparation method of 3-cyano-4-isopropoxy methyl benzoate
  • Preparation method of 3-cyano-4-isopropoxy methyl benzoate

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Embodiment

[0017] 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.

[0018] 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 3-cyano-4-isopropoxy methyl benzoate. The preparation method comprises the following steps: step I, preparing 3-aldehyde-4-methyl hydroxybenzoate from methyl p-hydroxybenzoate; step II, preparing 3-cyano-4-methyl hydroxybenzoate from the 3-aldehyde-4-methyl hydroxybenzoate; and step III, preparing the 3-cyano-4-isopropoxy methyl benzoate from the 3-cyano-4-methyl hydroxybenzoate. The preparation method of the 3-cyano-4-isopropoxy methyl benzoate provided by the invention has the advantages: (1) the use of cuprous cyanide of highly-toxic cyanide in the previous process is avoided, and the method is more suitable for industrialization; (2) the cyano is prepared from the aldehyde, so that high efficiency and directness can be realized, and mass production can be realized; and (3) all raw materials are cheap and easy to get, and the cost advantage is apparent.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a preparation method of 3-cyano-4-isopropoxymethyl benzoate. Background technique [0002] The traditional process for preparing methyl 3-cyano-4-isopropoxybenzoate 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-isopropoxy methyl benzoate, aim 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-isopropoxymethyl benzoate, comprising the steps: [0007] 1) Add magnesium chloride, triethylamine, paraformaldehyde, and dichlorometh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/57C07C253/30
CPCC07C67/313C07C253/00C07C253/30C07C255/57C07C69/76
Inventor 池永贵黄轩
Owner SUZHOU BLUEHILL BIOPHARMA CO LTD
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