5-Pyrimidinecarbonyl chloride, 4,6-dichloro- (9CI) synthesis

Yield:87600-97-3 100%

Reaction Conditions:

with sulfuryl dichloride;2,2'-azobis(isobutyronitrile) in tetrachloromethane at 80; for 4.5 h;

Steps:

24.1 Step 1) 4,6-dichloropyrimidine-5-carbonyl chloride

To a solution of 4,6-dichloropyrimidin-5-carbaldehyde (10 g, 56.50 mmol) in carbon tetrachloride (100 mL) were added sulfuryl chloride (11.44 g, 84.75 mmol) and 2,2-azobis(2-methylpropionitrile) (0.464 g, 2.83 mmol). The mixture was stirred at 80° C. for 4.5 hours, then cooled to room temperature and filtered. The filtrate was concentrated in vacuo and the residue was dried under a reduced pressure to obtain the title compound as a yellow colloid (12.22 g, yield: 100%).

References:

US2015/87658,2015,A1 Location in patent:Paragraph 0681