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Production method of 2-fluorine-4-nitrobenzonitrile

A technology of nitrobenzonitrile and clean production, which is applied in the direction of cyanide reaction preparation and organic chemistry. rate-boosting effect

Inactive Publication Date: 2014-04-02
CHANGZHOU VOCATIONAL INST OF ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] First, the amount of waste liquid generated at this stage is relatively large. For every 1T of 2-fluoro-4-nitrobromobenzene, 20-30 tons of acidic waste liquid will be produced. Such a large amount of waste liquid will cause environmental protection pressure to be worrying. ;
[0008] The second is that in this stage, refrigeration equipment is required to control the reaction temperature at 0-5°C, and the production energy consumption is relatively high

Method used

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  • Production method of 2-fluorine-4-nitrobenzonitrile
  • Production method of 2-fluorine-4-nitrobenzonitrile

Examples

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example 1

[0027] The preparation of example 1,2-fluoro-4-nitroaniline

[0028] Put 300L of industrial alcohol, 187.5L of 28% ammonia water, 6.8Kg of cuprous oxide and 120Kg of 3,4-difluoronitrobenzene into the high-pressure reactor, mix the above materials, raise the temperature to 120°C and control the pressure of the reactor at 1.7 MPa, heat preservation reaction for 18 hours, GC tracking reaction is basically over; after cooling down, the material is pressed into water, and 113.0Kg of yellow solid 2-fluoro-4-nitroaniline crude product is precipitated, the filter cake is washed and dried for later use, and its content is 99.61 %(GC).

[0029] Example 2, (1), put 250.0L of hydrobromic acid and 13.0Kg of copper powder into a 1000L reactor, stir and heat up to 100°C, keep warm for 3h, then cool down to 55°C; add 75.0L of Water, 56.2Kg of 2-fluoro-4-nitroaniline prepared in Example 1, and 100.0L of dichloroethane were added and kept at 55°C for 2 hours, and then 38.0Kg of 70.0L aqueous ...

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Abstract

The invention discloses a production method of 2-fluorine-4-nitrobenzonitrile, and particularly relates to a cleaning production method for improving the 2-fluorine-4-nitrobenzonitrile capable of being used as a drug intermediate of a tyrosine kinase irreversible inhibitor and a protein kinase inhibitor at a diazotization bromination reaction stage. A few defects exist at the traditional diazotization bromination reaction stage; one defect is that the amount of waste liquor generated at the stage is relatively large, and 20-30 T of acid waste liquor can be concomitantly generated when every 1 T of 2-fluorine-4-nitrobenzonitrile is generated; one defect is that the reaction temperature needs to be controlled between 0 DEG C and 5 DEG C by using refrigeration equipment at the stage, and the production energy consumption is relatively high. The invention aims at providing the clean production method of 2-fluorine-4-nitrobenzonitrile. The cleaning production method disclosed by the invention can effectively reduce the amount of the waste liquor generated by reaction at the diazotization bromination reaction stage and can increase the reaction temperature at the stage from 0-5 DEG C to 40-80 DEG C, thereby reducing the reaction energy consumption.

Description

technical field [0001] The invention relates to a production method of 2-fluoro-4-nitrobenzonitrile, in particular to a 2-fluoro-4-nitrobenzonitrile that can be used as a drug intermediate for tyrosine kinase irreversible inhibitors and protein kinase inhibitors A clean production method improved in the diazotization bromination reaction stage of benzonitrile. Background technique [0002] The English name of 2-fluoro-4-nitrobenzonitrile is 2-Fluoro-4-nitrobenzonitrile, and its molecular formula is C7H3FN2O2. It is a pharmaceutical intermediate and a pharmaceutical intermediate that can be used as an irreversible inhibitor of tyrosine kinase , the inhibitor can be used to treat diseases such as cancer, atherosclerosis, restenosis, endometriosis or psoriasis. [0003] At present, for several methods of synthesizing 2-fluoro-4-nitrobenzonitrile, please refer to the invention patent "Synthesis of a 2-fluoro-4-nitrobenzonitrile" published by Zhao Haoyu et al. on February 17, 20...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/50C07C253/14
Inventor 赵昊昱刘媛蒋涛吕潇
Owner CHANGZHOU VOCATIONAL INST OF ENG
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