4-CHLORO-2-(CHLOROMETHYL)PYRIMIDINE synthesis

Yield:-

Reaction Conditions:

with N-chloro-succinimide;2,2'-azobis(isobutyronitrile) in tetrachloromethane at 100; for 30 h;Inert atmosphere;Sealed tube;

Steps:

Preparation of 4-chloro-2-(chloromethyl)pyrimidine

The solution of 578 4-chloro-2-methylpyrimidine (3 g, 23.34 mmol), 579 1-chloropyrrolidine-2,5-dione (9.35 g, 70.01 mmol) and 580 azobisisobutyronitrile (766 mg, 4.67 mmol) in 581 carbon tetrachloride (30 mL) was sealed and stirred at 100° C. for 30 hours under a N₂ atmosphere. The reaction mixture was cooled to 20° C. and concentrated. The crude mixture was purified by flash chromatography with petroleum ether/ethyl acetate to give 582 4-chloro-2-(chloromethyl)pyrimidine.

References:

US2019/194189,2019,A1 Location in patent:Paragraph 0721-0722