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Method for preparing 1,1,3-trichloroacetone through high-selectivity chlorination of acetone

A high-selectivity, trichloroacetone technology, applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of poor synthesis technology, low preparation efficiency, and complicated operation process.

Active Publication Date: 2018-01-19
ANHUI COSTAR BIOCHEM CO LTD
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  • 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 relati

Method used

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  • Method for preparing 1,1,3-trichloroacetone through high-selectivity chlorination of acetone
  • Method for preparing 1,1,3-trichloroacetone through high-selectivity chlorination of acetone
  • Method for preparing 1,1,3-trichloroacetone through high-selectivity chlorination of acetone

Examples

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Example Embodiment

[0028] Example 1:

[0029] A method for preparing 1,1,3-trichloroacetone by highly selective chlorination of acetone, the preparation method comprising the following steps:

[0030] (1) Add 90 g of acetone to the container, add 1 g of triethylamine under stirring, then add 0.5 g of water, and control the temperature at 30° C. to feed chlorine gas to carry out the first chlorination stage;

[0031] (2) When the content of monochloroacetone in the reaction solution is lower than 1%, add alcohol compounds, and control the temperature to be 30° C. to carry out the second chlorination stage;

[0032] (3) When the dichloroacetone in the reaction solution is completely consumed, the reaction is stopped, air is blown in to blow out residual chlorine gas, and the solvent is removed by distillation under reduced pressure to obtain 1,1,3-trichloroacetone.

Example Embodiment

[0033] Example 2:

[0034] A method for preparing 1,1,3-trichloroacetone by highly selective chlorination of acetone, the preparation method comprising the following steps:

[0035] (1) Add 105g of acetone in the container, add 3g of triethylamine under stirring conditions, then add 3g of water, control the temperature at 60°C and feed chlorine gas to carry out the first chlorination stage;

[0036] (2) When the content of monochloroacetone in the reaction solution is lower than 1%, add an alcohol compound, and control the temperature to be 50° C. to carry out the second chlorination stage;

[0037] (3) When the dichloroacetone in the reaction solution is completely consumed, the reaction is stopped, air is blown in to blow out residual chlorine gas, and the solvent is removed by distillation under reduced pressure to obtain 1,1,3-trichloroacetone.

Example Embodiment

[0038] Example 3:

[0039] A method for preparing 1,1,3-trichloroacetone by highly selective chlorination of acetone, the preparation method comprising the following steps:

[0040] (1) Add 100 g of acetone to the container, add 1 g of triethylamine under stirring, then add 2 g of water, and control the temperature at 40° C. to feed chlorine to carry out the first chlorination stage;

[0041] (2) When the content of monochloroacetone in the reaction solution is lower than 1%, add alcohol compounds, and control the temperature to be 35° C. to carry out the second chlorination stage;

[0042] (3) When the dichloroacetone in the reaction solution is completely consumed, the reaction is stopped, air is blown in to blow out 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 through highly selective 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 Chinese published patent application CN106542979A, aiming at...

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Application Information

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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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