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Synthesis method of 4-chloro-2-butanone

A synthesis method and technology of butanone, applied in the field of 4-chloro-2-butanone synthesis, can solve problems such as waste, low process yield, unsuitable for industrial production, etc., and achieve convenient operation, simple process conditions and good market prospects Effect

Inactive Publication Date: 2014-02-05
ANHUI LANGXI LIANKE IND
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  • Summary
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing technology for preparing 4-chloro-2-butanone is to synthesize 4-hydroxyl-2-butanone and thionyl chloride in n-hexane. The yield of this process is low, and the n-hexane introduced has some Certain waste, not suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Step 1: Add 50g of 4-hydroxy-2-butanone solution into a 500ml four-necked bottle, and cool down to -5°C;

[0015] Step 2: Add 82g of thionyl chloride solution dropwise to the four-necked bottle, keep it warm at room temperature for 2 hours after dropping, raise the temperature to 60°C and keep it warm for 0.5 hour, then cool to room temperature;

[0016] The third step: wash the pH value of the solution in the previous step to 7 with 5 wt % sodium bicarbonate solution, and then obtain 47 g of 4-chloro-2-butanone product under reduced pressure.

Embodiment 2

[0018] Step 1: Add 50g of 4-hydroxy-2-butanone solution into a 500ml four-necked bottle, and cool down to -5°C;

[0019] Step 2: Add 82g of thionyl chloride solution dropwise to the four-necked bottle, keep it warm at room temperature for 2.5 hours after dropping, raise the temperature to 60°C and keep it warm for 0.9 hours, then cool to room temperature;

[0020] The third step: wash the pH value of the solution in the previous step to 7 with 5 wt % sodium bicarbonate solution, and then obtain 48 g of 4-chloro-2-butanone product under reduced pressure.

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Abstract

The invention discloses a synthesis method of 4-chloro-2-butanone. The method comprises the following steps: adding a 4-hydroxyl-2-butanone solution in a four-neck bottle of 500 ml and cooling to 5 DEG C below zero; dropwise adding a thionyl chloride solution into the four-neck bottle, preserving the heat for 2-3 hours at the room temperature after the thionyl chloride solution is dropwise added, heating to 60 DEG C and preserving the heat for 0.5-1 hour, and then cooling to the room temperature; washing the solution of the previous step by using 5wt% sodium bicarbonate until the pH (potential of Hydrogen) value is 7 and then decompressing to obtain the 4-chloro-2-butanone product. According to the method, the synthesis yield can be further improved while the use of the solvent is reduced, the technological conditions are simple and convenient, fewer pieces of chemical equipment are used, the flow is short, and the synthesis method is suitable for industrial production and thus has broad market space.

Description

technical field [0001] The invention belongs to the technical field of chemical preparation, and in particular relates to a synthesis method of 4-chloro-2-butanone. Background technique [0002] 4-Chloro-2-butanone is an intermediate commonly used in organic synthesis and is widely used in many chemical synthesis fields. The existing technology for preparing 4-chloro-2-butanone is to synthesize 4-hydroxyl-2-butanone and thionyl chloride in n-hexane. The yield of this process is low, and the n-hexane introduced has some Certain waste is not suitable for industrialized production. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a synthesis method of 4-chloro-2-butanone with simple process conditions, short process flow, high synthesis rate and easy industrial production. [0004] For solving above technical problem, technical scheme of the present invention is: a kind of 4-chloro-2-butanone synthetic method is ch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/63C07C49/16
CPCC07C45/63C07C49/16
Inventor 杨成超
Owner ANHUI LANGXI LIANKE IND
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