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US 11,858,873 B2Granted
Method for continuously synthesizing propellane compound
AssigneeJilin Asymchem Laboratories Co., Ltd.
InventorsHao Hong, Enxuan Zhang, Jiangping Lu, Fuliang Wei, Sihang Yang
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Abstract
Disclosed is a method for continuously synthesizing a propellane compound. The method includes the following steps: using 1,1-dibromo-2,2-bis(chloromethyl)cyclopropane or a derivative thereof as a raw material to form a ring with a lithium metal agent by a continuous reaction, so as to synthesize the propellane compound. A technical scheme of the present disclosure is applied, and a continuous reaction device is used.
Claims7
A method for continuously synthesizing a propellane compound, wherein the method comprises the following step:
- using 1,1-dibromo-2,2-bis(chloromethyl)cyclopropane or a derivative thereof as a raw material to form a ring with a lithium metal agent by a continuous reaction, so as to synthesize the propellane compound;
- the continuous reaction is carried out in a continuous stirred tank reactor;
- the continuous stirred tank reactor comprises a first-stage continuous stirred tank reactor, a second-stage continuous stirred tank reactor and a third-stage continuous stirred tank reactor which are connected in series;
- the 1,1-dibromo-2,2-bis(chloromethyl)cyclopropane or the derivative thereof is dissolved in a first solvent to obtain solution A, and the lithium metal agent is dissolved in a second solvent to obtain solution B, and the solution A and the solution B are added to the continuous stirred tank reactor by an automatic feeding system for the continuous reaction;
- in the solution A, the molar concentration of the 1,1-dibromo-2,2-bis(chloromethyl) cyclopropane or the derivative thereof is 0.5 to 3.0 M;
- in the solution B, the molar concentration of the lithium metal agent is 1.0 M to 3.0 M;
- the feeding ratio of the solution A to the solution B is 1:2.0 to 1:3.0;
- in the first stage continuous stirred tank reactor, the reaction temperature is −51° C. to −75° C., and the reaction time is 20 to 40 min;
- in the second stage continuous stirred tank reactor, the reaction temperature is −5° C. to 5° C., and the reaction time is 30 to 60 min;
- and
- in the third stage continuous stirred tank reactor, the reaction temperature is −5° C. to 5° C., and the reaction time is 30 to 60 min;
- the 1,1-dibromo-2,2-bis(chloromethyl)cyclopropane or a derivative thereof has the following structure:
- wherein R1 and R2 each independently are —CH3 or —C2H5.
10 more elements
Dependencies are inferred from the claim text.