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Separation method of by-products from preparation of 4-chloro-2-(trifluoroacetyl)-aniline hydrochloride

A technology of aniline hydrochloride and trifluoroacetyl, which is applied in the field of separation of by-products of 4-chloro-2-aniline hydrochloride, can solve the problems of high pressure on environmental protection, large consumption of liquid alkali, and high production costs, and achieves The effect of reducing environmental pressure, simple production equipment, and reducing pollutant emissions

Inactive Publication Date: 2018-11-16
JIANGSU SHAXING CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] 4-Chloro-(2-trifluoroacetyl)-aniline hydrochloride is an important intermediate for the preparation of efavirenz. Currently, the preparation of 4-chloro-(2-trifluoroacetyl)-aniline hydrochloride uses N-pentamyl Acyl-4-(2-trifluoroacetyl)-aniline is used as a raw material, prepared by deprotecting groups of acetic acid and hydrochloric acid, and pivalic acid is generated at the same time, forming a mixed acid system of hydrochloric acid, acetic acid and pivalic acid. The mixed acid is an azeotropic system. There is no report on the treatment method of the mixed acid system, and the biochemical treatment method is generally used, but the biochemical treatment is used after the pH value of the system is neutralized by liquid alkali neutralization in the sewage treatment center, which needs to consume a large amount of liquid alkali and generate more by-products. Product Sodium chloride, sodium acetate and other by-products
This puts a lot of pressure on environmental protection and high production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 500ml of solvent into the reactor, put in 300ml of 1,2-dichloroethane, use a 40cm packed column, heat up and distill under normal pressure, control the temperature rise rate to distill out liquid stratification, and ensure that the output of the upper aqueous phase is controlled at 40-50ml / min, the reflux flow rate of the lower layer is controlled at 80-100ml / min, after the top temperature is 80-82°C, after the anhydrous phase is distilled out, the dehydration ends, and the hydrochloric acid content in the water phase is detected to be 20.5%, and the acetic acid content is 3.5%; continue to recover two Ethyl chloride ends at a top temperature of 117°C, the content of dichloroethane is 97.4%, and the content of acetic acid is 2.3%.

[0019] The residue was rectified under reduced pressure, and the 50-60°C fraction at -0.095MPa was collected, and 96.7% of acetic acid was detected, and pivalic acid was recovered by continuing to raise the temperature and distilled, wit...

Embodiment 2

[0021] Add 500ml of solvent into the reactor, put in 400ml of 1,1-dichloroethane, use a 40cm packed column, heat up and distill at normal pressure, control the temperature rise rate to distill out liquid stratification, and ensure that the output of the upper aqueous phase is controlled at 40-50ml / min, the reflux flow rate of the lower layer is controlled at 80-100ml / min, after the top temperature is 80-82°C, after the anhydrous phase is distilled out, the dehydration is completed, and the hydrochloric acid content in the water phase is detected to be 21.5%, and the acetic acid content is 1.5%; continue to recover two Ethyl chloride ends at a top temperature of 115°C, and the GC content of dichloroethane is 98.4%, and the content of acetic acid is 1.2%.

[0022] The residue was rectified under reduced pressure, and the 50-60°C fraction at -0.095MPa was collected, and the acetic acid was detected to be 96.7%, and the pivalic acid was recovered by continuous heating distillation...

Embodiment 3

[0024] Add 600ml of solvent into the reactor, put in 400ml of 1,2-dichloropropane, use a 40cm packing column, heat up and distill at normal pressure, control the temperature rise rate to distill out liquid stratification, and ensure that the output of the upper aqueous phase is controlled at 40-50ml / Min, the reflux flow rate of the lower layer is controlled at 90ml / min, after reaching the top temperature of 80°C, after the anhydrous phase is distilled out, the dehydration is completed, and the hydrochloric acid content in the water phase is detected to be 22.5%, and the acetic acid content is 1.2%; continue to recover dichloropropane to the top temperature After finishing at 110°C, the GC content of dichloropropane was 98.4%, and the content of acetic acid was 1.1%.

[0025] The residue was rectified under reduced pressure, and the 50-60°C fraction at -0.095MPa was collected, and 97.2% of acetic acid was detected, and the pivalic acid was recovered by continuous heating distil...

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Abstract

The invention provides a separation method of by-products from preparation of 4-chloro-2-(trifluoroacetyl)-aniline hydrochloride and specifically relates to the technical field of compound preparationmethods. The separation method comprises a Step a and a Step b: Step a, a reaction solvent is added into a mixed acid system for separation, reflux and dehydration to separate a hydrochloric acid aqueous solution, and then the reaction solvent is recovered, wherein the reaction solvent is dichloroethane or dichloropropane; Step b, residues undergo underpressure distillation to respectively separate and recover acetic acid and pivalic acid. The production equipment is simple, and operation is simple; emission of pollutants is reduced, and environmental protection pressure is decreased; the recovered hydrochloric acid and acetic acid can be directly used in a reaction, and with repeated use, production cost is reduced; and the separation method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of compound preparation methods, and in particular relates to a separation method for preparing 4-chloro-2-(trifluoroacetyl)-aniline hydrochloride by-products. Background technique [0002] 4-Chloro-(2-trifluoroacetyl)-aniline hydrochloride is an important intermediate for the preparation of efavirenz. Currently, the preparation of 4-chloro-(2-trifluoroacetyl)-aniline hydrochloride uses N-pentamyl Acyl-4-(2-trifluoroacetyl)-aniline is used as a raw material, prepared by deprotecting groups of acetic acid and hydrochloric acid, and pivalic acid is generated at the same time, forming a mixed acid system of hydrochloric acid, acetic acid and pivalic acid. The mixed acid is an azeotropic system. There is no report on the treatment method of the mixed acid system, and the biochemical treatment method is generally used, but the biochemical treatment is used after the pH value of the system is neutralized by liquid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/045C07C17/383C07C53/08C07C53/126C07C51/44
CPCC07C17/383C07C51/44C07C19/045C07C53/08C07C53/126
Inventor 潘江平王宏胜刘海军刘西统
Owner JIANGSU SHAXING CHEM
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