Micro-reaction system and method for preparing 2-methyl-4-amino-5-aminomethyl pyrimidine
AssigneeFudan University
InventorsFener Chen, Meifen Jiang, Dang Cheng, Minjie Liu, Huashan Huang
Life of this patent
Estimating the term…
Abstract
A micro-reaction system and a method for preparing 2-methyl-4-amino-5-aminomethyl pyrimidine. A Raney nickel catalyst is modified with formalin, and the modified Raney nickel catalyst is filled into a micro-channel reactor of the micro-reaction system. A substrate solution containing 2-methyl-4-amino-5-cyanopyrimidine and a base and hydrogen are transported to the micro-mixer and the micro-channel reactor in sequence for continuous catalytic hydrogenation to obtain 2-methyl-4-amino-5-aminomethyl pyrimidine.
Claims10
A method for preparing 2-methyl-4-amino-5-aminomethyl pyrimidine using a micro-reaction system, the micro-reaction system comprising a micro-mixer and a micro-channel reactor communicated in sequence;
- and the method comprising:
- (1) modifying a Raney nickel catalyst with formalin to obtain a modified Raney nickel catalyst;
- and filling the micro-channel reactor with the modified Raney nickel catalyst;
- (2) transporting a substrate solution containing 2-methyl-4-amino-5-cyanopyrimidine and a base and hydrogen to the micro-mixer followed by mixing;
- allowing the reaction mixture flowing out of the micro-mixer to enter the micro-channel reactor;
- and subjecting the reaction mixture to catalytic hydrogenation;
- 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-aminomethyl pyrimidine;
- wherein the 2-methyl-4-amino-5-aminomethyl pyrimidine is shown in formula (I), and the 2-methyl-4-amino-5-cyanopyrimidine is shown in formula (II);
- and the catalytic hydrogenation is shown in the following reaction scheme:
A micro-reaction system for preparing 2-methyl-4-amino-5-aminomethyl pyrimidine, comprising:
- a feed pump;
- a gas mass flow meter equipped with a flow controller;
- a micro-mixer;
- a micro-channel reactor;
- a condenser;
- a gas-liquid separator;
- and
- a back pressure valve;
- wherein the micro-mixer is provided with two inlets;
- one inlet of the micro-mixer is connected to the gas mass flow meter, and the other inlet of the micro-mixer is connected to the feed pump;
- an outlet of the micro-mixer is connected to an inlet of the micro-channel reactor, and an outlet of the micro-channel reactor is connected to an inlet of the condenser;
- a top of the gas-liquid separator is provided with a first port, a second port and a third port;
- an outlet of the condenser is connected to the first port;
- the second port is configured to introduce nitrogen to provide a pressure in the gas-liquid separator;
- a pressure of the nitrogen is 0.1-4.5 MPa;
- the back pressure valve is connected to the third port, and a back pressure of the back pressure valve is 0.1-4 MPa;
- and a pressure of the nitrogen is 0.2-0.5 MPa larger than a back pressure value set by the back pressure valve;
- the micro-channel reactor is filled with a formalin-modified Raney nickel catalyst;
- the feed pump and the gas mass flow meter are configured to transport a substrate solution containing 2-methyl-4-amino-5-cyanopyrimidine and hydrogen to the micro-mixer, respectively;
- the micro-mixer is configured for mixing the substrate solution with hydrogen obtain a reaction mixture;
- the reaction mixture flowing out of the micro-mixer enters into the micro-channel reactor and undergoes a catalytic hydrogenation;
- after flowing out of the micro-channel reactor, the reaction mixture is condensed in the condenser, and then enters the gas-liquid separator, a waste gas generated in the gas-liquid separator is discharged through the third port and the back pressure valve;
- and the reaction mixture is discharged through an outlet provided 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-aminomethyl pyrimidine;
- wherein the 2-methyl-4-amino-5-aminomethyl pyrimidine is shown in formula (I):
- and the 2-methyl-4-amino-5-cyanopyrimidine is shown in formula (II):
Dependencies are inferred from the claim text.