A kind of method for preparing 1,1,3-trichloroacetone by chlorination of acetone

A technology of trichloroacetone and acetone, which is applied in the field of folic acid intermediate synthesis, can solve the problems of poor synthesis technology, low preparation efficiency, and low product selectivity, and achieve the effect of avoiding the formation of by-products

Active Publication Date: 2020-06-05
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although the method for preparing 1,1,3-trichloroacetone provided by the prior art can achieve a certain yield, there are still relatively poor synthesis technology, low preparation efficiency, low selectivity of the obtained product, and cumbersome operation process Defects

Method used

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  • A kind of method for preparing 1,1,3-trichloroacetone by chlorination of acetone

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Embodiment 1

[0028] A method for preparing 1,1,3-trichloroacetone by chlorination of acetone, the preparation method comprising the following steps:

[0029] (1) Add 90g of acetone into the container, add 1g of triethylamine under stirring conditions, then add 0.5g of water, and control the temperature at 30°C to pass chlorine gas to carry out the first chlorination stage;

[0030] (2) When the content of monochloroacetone in the reaction solution is lower than 1%, add alcohol compounds, and control the temperature at 30°C for the second chlorination stage;

[0031] (3) When the dichloroacetone in the reaction solution is completely consumed, the reaction is stopped, air is blown in to blow out the residual chlorine gas, and the solvent is removed by distillation under reduced pressure to obtain 1,1,3-trichloroacetone.

Embodiment 2

[0033] A method for preparing 1,1,3-trichloroacetone by chlorination of acetone, the preparation method comprising the following steps:

[0034] (1) Add 105g of acetone into the container, add 3g of triethylamine under stirring conditions, then add 3g of water, control the temperature at 60°C and pass chlorine gas to carry out the first chlorination stage;

[0035] (2) When the content of monochloroacetone in the reaction solution is lower than 1%, add alcohol compounds, and control the temperature at 50°C for the second chlorination stage;

[0036] (3) When the dichloroacetone in the reaction solution is completely consumed, the reaction is stopped, air is blown in to blow out the residual chlorine gas, and the solvent is removed by distillation under reduced pressure to obtain 1,1,3-trichloroacetone.

Embodiment 3

[0038] A method for preparing 1,1,3-trichloroacetone by chlorination of acetone, the preparation method comprising the following steps:

[0039] (1) Add 100g of acetone to the container, add 1g of triethylamine under stirring conditions, then add 2g of water, control the temperature at 40°C and pass chlorine gas to carry out the first chlorination stage;

[0040] (2) When the content of monochloroacetone in the reaction solution is lower than 1%, add alcohol compounds, and control the temperature at 35°C for the second chlorination stage;

[0041] (3) When the dichloroacetone in the reaction solution is completely consumed, the reaction is stopped, air is blown in to blow out the residual chlorine gas, and the solvent is removed by distillation under reduced pressure to obtain 1,1,3-trichloroacetone.

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Abstract

The invention relates to the technical field of synthesis of a folic acid intermediate, in particular to a method for preparing 1,1,3-trichloroacetone through high-selectivity chlorination of acetone.The method comprises the process steps as follows: firstly, acetone is taken as a raw material and subjected to staged catalytic chlorination of chlorine, an amine compound is taken as a catalyst tochlorinate acetone to a dichloroacetone stage, then, an alcohol compound is added to serve as a solvent, water is added to adjust the reaction process, 1,1,3-trichloroacetone is prepared through deepchlorination, and the yield of the method is up to 90% or above. With the adoption of the technical scheme, the defects that existing preparation methods for 1,1,3-trichloroacetone have poorer synthesis technological level, low preparation efficiency and complex operation process and obtained products are low in selectivity can improved to a certain extent.

Description

technical field [0001] The invention relates to the technical field of folic acid intermediate synthesis, in particular to a method for preparing 1,1,3-trichloroacetone by chlorination of acetone. Background technique [0002] 1,1,3-Trichloroacetone is a colorless, transparent liquid with a strong pungent odor. It is an important chemical intermediate widely used in organic synthesis, medicine, pesticides, spices and dyes, etc. , the main application is for the synthesis of folic acid. [0003] At present, the main methods for preparing 1,1,3-trichloroacetone include acetone direct chlorination method, acetone indirect chlorination method, acetone catalytic chlorination method and refining method. The direct chlorination method of acetone uses chlorine gas for chlorination, the reaction time is long, and the selectivity of 1,1,3-trichloroacetone is poor and difficult to separate. [0004] In the Chinese published patent application CN106542979A, aiming at obtaining a kind ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/63C07C49/16
Inventor 王红伟王佳傅胜辉杨红军张明祥陈军谢珊
Owner ANHUI COSTAR BIOCHEM CO LTD
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