2,4-DIOXO-1,2,3,4-TETRAHYDROPYRIMIDINE-5-SULFONYL CHLORIDE synthesis

Yield:28485-18-9 92.3%

Reaction Conditions:

with chlorosulfonic acid;thionyl chloride at 25 - 75; for 12.5 h;

Steps:

4.1.1. The synthesis of 2,4-dihydroxypyrimidine-5-sulfonyl chloride(1)

2, 4-dihydroxypyrimidine (6 g, 53.57 mmol) and thionylchloride(SOCl2) (10 mL, 89.22 mmol) were added to a 100 mL reaction askat 25C. After chlorosulfonic acid (HSO3Cl) (16 g, 138.05 mmol) wasadded at room temperature for 1.5 h. The reaction was stirred at60C for 4 h in an oil bath and then at 75C for 7 h. The reactionmixture was added to a mixture of ice and glacial acetic acid (1:1).The precipitate was precipitated and suction ltered, washedrepeatedly and dried at 50C to give compound 1 as white powder.Yield: 92.30%.

References:

Li, Xin-yang;Liang, Jing-wei;Mohamed O, Kamara;Zhang, Ting-jian;Lu, Guo-Qing;Meng, Fan-hao [European Journal of Medicinal Chemistry,2018,vol. 154,p. 267 - 279]