A kind of post-processing method for continuous synthesis of methyl 4-chloroacetoacetate
A technology of methyl acetate and chloroacetyl, which is applied in the post-treatment field of continuous synthesis of methyl 4-chloroacetoacetate, can solve the problems of unsatisfactory use requirements, poor washing effect, general treatment effect, etc., and achieve good washing effect, Ease of implementation and concise method
Active Publication Date: 2022-04-19
JIANGSU HENGAN CHEM
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[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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[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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The invention discloses a post-treatment method for continuously synthesizing methyl 4-chloroacetoacetate, which comprises the following steps: Step 1: using diketene, chlorine gas, methylene chloride and methanol as raw materials, and preparing it through chlorination and esterification reactions Containing the dichloromethane solution of 4-chloroacetoacetate methyl ester; Step 2: adding the dichloromethane solution containing 4-chloroacetoacetate methyl ester in the washing device, the aqueous solution and the organic solution are separated; Step 3: the organic solution is purified Distillation obtains the finished product of methyl 4-chloroacetoacetate. The inventive method is concise and easy to realize. The washing device proposed by the present invention can realize the continuous rapid water-washing process to the dichloromethane solution containing methyl 4-chloroacetoacetate. The water washing effect is good and the efficiency is high, which meets the current use requirements.
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°...
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IPC IPC(8): C07C67/46C07C67/58C07C67/54C07C69/72B01D11/04B01F23/43B01F27/192B01F27/80B01F27/92
CPCC07C67/46C07C67/58C07C67/54B01D11/0492B01F23/43B01F27/192B01F27/92B01F27/80C07C69/72
Inventor 王海根
Owner JIANGSU HENGAN CHEM