Microreactor and synthesis method for chlorination reaction of α-position hydrogen atom of α-dicarbonyl compound
A technology of dicarbonyl compound and chlorination reaction is applied in the chlorination reaction of α-position hydrogen atom of α-dicarbonyl compound, in the field of chemical synthesis, and can solve the problems of severe reaction exotherm, poor reaction selectivity, unsatisfactory yield and the like, To achieve the effect of less dosage, mild conditions and environmental friendliness
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[0020] The present application also provides a method for preparing the chlorinated compound of the α-position hydrogen atom of the α-dicarbonyl compound, that is, using the α-dicarbonyl compound and chlorine as raw materials, in a micropipe, the chlorination of the α-position hydrogen atom of the α-dicarbonyl compound is realized. The reaction can be carried out under solvent and solvent-free conditions. However, it is preferably carried out under solvent-free conditions. Specifically, the microreactor device is used to prepare the method for the chlorination of the α-position hydrogen atom of the α-dicarbonyl compound, comprising the following steps:
[0021] 1) prepare raw material α-dicarbonyl compound and chlorine for subsequent use; the molar ratio of described raw material α-dicarbonyl compound and chlorine is: 0.5:1~1:2;
[0022] 2) Feed the raw materials through different feed pumps according to a certain ratio, and react through the micro-reaction channel, the react...
Embodiment 1
[0025]
[0026] The temperature of the temperature control device was adjusted to 25°C, the system pressure was 1 to 2 atm, and under solvent-free conditions, the flow rate of the substrate α-acetyl-γ-butyrolactone was adjusted to 10mol / h, and the flow rate of chlorine was 10.5mol / h, The material is injected into the reaction system with a metering pump for reaction, and the reaction time is controlled to be 30s according to the reaction requirements. As the reaction progressed, the temperature at the reactor outlet gradually increased to 45°C, and the temperature at the outlet of line 2 increased to 35°C. The reaction was completed for 2h, and sampling was carried out for gas phase analysis. The reaction selectivity was 99.3%, and the quantitative yield was 98.6%.
Embodiment 2
[0028]
[0029] Adjust the temperature of the temperature control device to 15°C, and the system pressure to 1 to 2 atm. Under solvent-free conditions, adjust the flow rate of the substrate acetylacetone to 1 mol / h and the flow of chlorine gas to 1.0 mol / h, and use a metering pump to pump the material into the reaction. The reaction was carried out in the system, and the reaction time was controlled to be 20s according to the reaction requirements. As the reaction progressed, the temperature at the reactor outlet gradually increased to 35°C, and the temperature at the outlet of line 2 increased to 25°C. The reaction was completed for 1h, and sampling was carried out for gas phase analysis. The reaction selectivity was 83.1%, and the quantitative yield was 79.2%.
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