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Production method of 3-methyl-4-nitrobenzoate trichloronitrile butyl ester

A technology of trichloronitrile butyl nitrobenzoate and nitrobenzoic acid is applied in the preparation of carboxylic acid nitrile, chemical instruments and methods, preparation of organic compounds, etc., and can solve difficult separation, low product purity, and many impurities. and other problems to achieve the effect of reducing production cost and improving reaction yield

Active Publication Date: 2019-08-09
山东华科化工有限公司
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Problems solved by technology

In the prior art, the preparation process of the acylation unit 3-methyl-4-nitrobenzoyl chloride adopts 3-methyl-4-nitrobenzoic acid as a raw material, and phosphorus oxychloride (or phosphorus pentachloride) The reaction produces 3-methyl-4-nitrobenzoyl chloride, which has the problem of many impurities and difficult separation, and the product purity is relatively low

Method used

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  • Production method of 3-methyl-4-nitrobenzoate trichloronitrile butyl ester
  • Production method of 3-methyl-4-nitrobenzoate trichloronitrile butyl ester

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Embodiment 1

[0030] 1. Preparation of condensation unit 2,4,4-trichloro-4-formaldehyde solution butyronitrile

[0031] Enamel reaction kettle R1050, R1051, R1052, R1053, R1054, R1055, add chloral 1000Kg, acrylonitrile 600Kg, catalyst cuprous chloride 50Kg, heat up to 78~82℃, reflux for 24 hours for condensation reaction, after the reaction Cool to 35-40°C, the materials in R1050, R1051 and R1052 are transported to R1031, R1032 or R1034 through R1033, the materials in R1053, R1054 and R1055 are transported to R1035, R1036 or R1037 through R1038, and unreacted is recovered by vacuum distillation A mixture of acrylonitrile and chloral, repeated.

[0032] When the temperature rises to 100°C, the recovery is over, the temperature is lowered to 30°C, 1000Kg of sulfolane is added respectively, the materials in the kettle are transferred to R1003, R1004 and R1005, and the low boilers are further distilled to R1006 and R1007.

[0033] Cool the remaining materials in R1003, R1004 and R1005 to 30°C,...

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Abstract

The invention belongs to the technical field of fine chemistry, and relates to a production method of 3-methyl-4-nitrobenzoate trichloronitrile butyl ester. The production method comprises following steps: (1), cuprous chloride is taken as a catalyst, trichloroacetaldehyde and acrylonitrile are reacted at 65 to 95 DEG C to prepare 2, 4, 4-trichloro-4-formaldehyde butyronitrile; (2), formaldehyde,calcium hydrate, and 2, 4, 4-trichloro-4-formaldehyde butyronitrile are reacted at 30 to 70 DEG C so as to prepare 2, 4, 4-trichlorocyanbutanol; (3), 3-methyl-4 nitrobenzoic acid, pyridine, and thionyl chloride are reacted at 30 to 120 DEG C to prepare 3-methyl-4-nitro benzoyl chloride; and (4), 2, 4, 4-trichlorocyanbutanol and 3-methyl-4-nitro benzoyl chloride are reacted at 30 to 50 DEG C so asto obtain a finished product. The production method is capable of increasing the entire reaction yield, and reducing production cost; and is suitable for industrialized production.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a production method of 3-methyl-4-nitrobenzoic acid trichloronitrile butyl. Background technique [0002] 3-Methyl-4-nitrobenzoic acid trichloronitrile butyl ester is an important chemical intermediate, mainly used in the production of pharmaceuticals, pesticides, and intermediates in the production of dyes and photosensitive materials. At present, the production process of 3-methyl-4-nitrobenzoic acid trichloronitrile butyl ester can be divided into four units: condensation unit 2,4,4-trichloro-4-formaldehyde solution butyronitrile preparation process , the preparation process of the reduction unit 2,4,4-trichlorocyanobutanol, the preparation process of the acylation unit 3-methyl-4 nitrobenzoyl chloride, the esterification unit product 3-methyl-4 nitrobenzene Preparation procedure of trichlorocyanobutyl formate. [0003] At present, the preparation process ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/14C07C201/12C07C205/57C07C255/12
CPCC07C201/12C07C253/30C07C255/14C07C205/57C07C255/12C07C255/17
Inventor 周红霞程李中左俊坤陈厚松罗志峰陈国云
Owner 山东华科化工有限公司
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