Micro reaction system and method for preparing 2-methyl-4-amino-5-cyanopyrimidine using same
AssigneeFudan University
InventorsFener Chen, Meifen Jiang, Dang Cheng, Minjie Liu, Huashan Huang
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Abstract
Disclosed herein relates to pharmaceutical engineering, and more particularly to a micro reaction system and a method for preparing 2-methyl-4-amino-5-cyanopyrimidine using the same. An acetamidine hydrochloride solution and an (dimethylaminomethylene)malononitrile solution are separately pumped into the micro reaction system including a micromixer and an agitating microchannel reactor in communication at the same time for a continuous condensation-cyclization reaction to obtain 2-methyl-4-amino-5-cyanopyrimidine.
Claims11
A method for preparing 2-methyl-4-amino-5-cyanopyrimidine using a micro reaction system, the micro reaction system comprising a micromixer and an agitating microchannel reactor communicated in sequence, and the method comprising:
- (1) pumping an acetamidine hydrochloride solution and a (dimethylaminomethylene)malononitrile solution separately into the micromixer at the same time followed by mixing;
- (2) allowing the reaction mixture flowing out of the micromixer to enter the agitating microchannel reactor;
- and subjecting the reaction mixture to condensation-cyclization reaction;
- and
- (3) collecting the reaction mixture flowing out of the micro reaction system;
- and subjecting the reaction mixture to separation and purification to obtain a target product 2-methyl-4-amino-5-cyanopyrimidine;
- wherein the 2-methyl-4-amino-5-cyanopyrimidine is shown in formula (I);
- the acetamidine hydrochloride is shown in formula (II);
- the (dimethylaminomethylene)malononitrile is shown in formula (III);
- the condensation-cyclization reaction is shown in the following reaction scheme;
A micro reaction system for preparing 2-methyl-4-amino-5-cyanopyrimidine, comprising:
- a first pump;
- a second pump;
- a micromixer;
- an agitating microchannel reactor;
- a gas-liquid separator;
- and
- a back pressure valve;
- wherein the first pump is configured to feed an acetamidine hydrochloride solution;
- the second pump is configured to feed a (dimethylaminomethylene)malononitrile solution;
- a first inlet of the micromixer is connected to the first pump;
- a second inlet of the micromixer is connected to the second pump;
- an outlet of the micromixer is connected to an inlet of the agitating microchannel reactor;
- a top of the gas-liquid separator is provided with a first port, a second port and a third port;
- the first port is connected to an outlet of the agitating microchannel reactor;
- the second port is configured to introduce nitrogen to provide a pressure in the gas-liquid separator, where a pressure of the nitrogen is 0-2.5 MPa;
- the third port is connected to the back pressure valve;
- a back pressure of the back pressure valve is 0-2 MPa;
- and the pressure of the nitrogen is 0-0.5 MPa larger than a backpressure set by the back pressure valve;
- the acetamidine hydrochloride solution and the (dimethylaminomethylene)malononitrile solution are pumped into the micromixer at the same time through the first pump and the second pump, respectively;
- the reaction mixture flowing out of the micromixer enters the agitating microchannel reactor and undergoes a continuous condensation-cyclization reaction;
- the reaction mixture flowing out of the agitating microchannel reactor enters the gas-liquid separator;
- a gas in the gas-liquid separator is discharged through the third port and the back pressure valve;
- and the reaction mixture is discharged from an outlet at a bottom of the gas-liquid separator, collected and subjected to separation and purification to obtain a target product 2-methyl-4-amino-5-cyanopyrimidine;
- wherein the 2-methyl-4-amino-5-cyanopyrimidine is shown in formula (I):
- the acetamidine hydrochloride is shown in formula (II):
- and
- the (dimethylaminomethylene)malononitrile is shown in formula (III):
Dependencies are inferred from the claim text.