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Post-treatment method for continuously synthesizing methyl 4-chloroacetoacetate

A technology of methyl acetate and chloroacetyl, applied in the post-processing field of continuous synthesis of methyl 4-chloroacetoacetate, can solve the problems such as inability to meet use requirements, general processing effect, poor washing effect, etc., and achieves good washing effect, Good effect and easy to achieve effect

Active Publication Date: 2020-11-24
JIANGSU HENGAN CHEM
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Problems solved by technology

[0004] Now 4-chloroacetoacetate methyl ester in the post-processing after synthesis, the treatment effect is general, especially when the dichloromethane solution containing 4-chloroacetoacetate methyl ester is washed, the washing effect is not good, the efficiency is low, can not Meet current usage requirements

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  • Post-treatment method for continuously synthesizing methyl 4-chloroacetoacetate
  • Post-treatment method for continuously synthesizing methyl 4-chloroacetoacetate
  • Post-treatment method for continuously synthesizing methyl 4-chloroacetoacetate

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Embodiment

[0026] Reference attached Figure 1-3 , the present invention will be described in further detail below in conjunction with accompanying drawing:

[0027] A post-processing method for continuously synthesizing methyl 4-chloroacetoacetate, comprising the steps:

[0028] Step 1: using diketene, chlorine, dichloromethane and methanol as raw materials, through chlorination and esterification to obtain a dichloromethane solution containing methyl 4-chloroacetoacetate;

[0029] Step 2: adding a dichloromethane solution containing methyl 4-chloroacetoacetate into a water washing device to separate the aqueous solution from the organic solution;

[0030] Step 3: The organic solution is rectified to obtain the finished product of methyl 4-chloroacetoacetate.

[0031] The water washing device comprises a closed tower still 100, and the tower still 100 is arranged along the plumb direction, and the A shower nozzle 300 and the B shower nozzle that feeds into the dichloromethane solution...

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Abstract

The invention discloses a post-treatment method for continuously synthesizing methyl 4-chloroacetoacetate. The method comprises the following steps of 1, carrying out chlorination reaction and esterification reaction on diketene, chlorine, dichloromethane and methanol serving as raw material agents to obtain a dichloromethane solution containing methyl 4-chloroacetoacetate; step 2, adding the dichloromethane solution containing methyl 4-chloroacetoacetate into a washing device, and separating an aqueous solution from an organic solution; and step 3, rectifying the organic solution to obtain amethyl 4-chloroacetoacetate finished product. The method is simple and clear and convenient to implement, the washing device provided by the invention can realize continuous and rapid washing treatment on the dichloromethane solution containing methyl 4-chloroacetoacetate, the washing effect is good, the efficiency is high, and the current use requirements are met.

Description

technical field [0001] The invention relates to the field of chemical preparation, in particular to a post-treatment method for continuously synthesizing methyl 4-chloroacetoacetate. Background technique [0002] Methyl 4-chloroacetoacetate is a colorless light yellow liquid, which is a good intermediate for pharmaceutical synthesis and is mainly used to produce oxiracetam, which is a drug for treating cerebrovascular diseases. [0003] At present, the main conventional production method of methyl 4-chloroacetoacetate in industrial production is: batch production, first dissolving diketene in a solvent, and cooling it to -30°C ~ -10°C, starting stirring, and pouring it into the reaction kettle Introduce a certain amount of chlorine gas at a certain flow rate, keep it warm at -30°C to -10°C for 1 to 2 hours, drop a certain amount of methanol into it after the chlorination reaction is completed, control the reaction temperature at 0 to 5°C, and raise the temperature to 20-25°...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/46C07C67/58C07C67/54C07C69/72B01D11/04B01F3/08B01F7/16B01F7/24
CPCC07C67/46C07C67/58C07C67/54B01D11/0492B01F23/43B01F27/192B01F27/92B01F27/80C07C69/72
Inventor 王海根
Owner JIANGSU HENGAN CHEM
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