Method and device for continuously synthesizing cyclopropane compounds
AssigneeAsymchem Laboratories (Tianjin) Co., Ltd.
InventorsHao Hong, Jiangping Lu, Xichun Feng, Xingfang Sun, Feng Zhang
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Abstract
The present disclosure discloses a method and a device for continuously synthesizing cyclopropane compounds. The method includes the following steps: continuously performing a synthetic reaction of a diazomethane precursor in a first reactor, the reaction product of the first reactor flowing into a separator for stratification, the organic phase obtained by stratification overflowing into a second reactor, continuously consuming the diazomethane precursor in a second reactor to prepare diazomethane and performing an electron-rich monoolefin cyclopropanation reaction in situ so as to obtain the cyclopropane compound.
Claims17
A method for continuously synthesizing a cyclopropane compound comprising the following steps:
- continuously performing a synthetic reaction of a diazomethane precursor in a first reactor, the reaction product of the first reactor flowing into a separator for stratification, the organic phase obtained by stratification overflowing into a second reactor, continuously consuming the diazomethane precursor in the second reactor to prepare diazomethane and performing an electron-rich monoolefin cyclopropanation reaction on diazomethane in situ so as to obtain the cyclopropane compound;
- the method for continuously synthesizing the cyclopropane compound further comprises a post-treatment step for the product of the second reactor;
- an electron-rich monoolefin compound and a palladium-containing catalyst are dissolved in tetrahydrofuran and continuously pumped into the second reactor by a fourth feed pump, while an aqueous potassium hydroxide solution is continuously pumped into the second reactor by a fifth feed pump;
- the electron-rich monoolefin compound has the following structure:
- wherein R1 represents hydrogen, t-butyl oxycarbonyl or carbobenzoxy;
- R2 represents hydrogen, phenyl, methyl or pyridyl;
- and R3 represents hydrogen, methyl or ethyl.
Dependencies are inferred from the claim text.