1H-1,2,4-Triazole-3-sulfonyl chloride, 1-[(dimethylamino)sulfonyl]- synthesis

Yield:171967-86-5 95%

Reaction Conditions:

with trichloroisocyanuric acid in dichloromethane;water at -10 - 20; for 2 h;

Steps:

4 Example 4: Preparation of 1-(N,N-dimethylaminosulfonyl)-1H-1,2,4-triazole-3-sulfonyl chloride

At room temperature, 3-((1-(N,N-dimethylaminosulfonyl)-1H-1,2,4-triazol-3-yl)disulfanyl)-N,N-dimethyl Base-1H-1,2,4-triazole-1-sulfonamide (A, 5.0kg, 12.07mol), dichloromethane (30L) and water (5L) were added to a 100L stirred reaction kettle, and at -10 After stirring evenly at , slowly add TCCA (5.61kg, 24.14mol) in batches, after adding, continue stirring at -10 for 1 hour, place the reaction solution at room temperature and continue stirring for 1 hour,The reaction of the starting material was monitored by HPLC for completion. At room temperature, the reaction solution was allowed to stand for 10 minutes, the lower layer liquid was separated, the residual chlorine gas was removed by bubbling with nitrogen, and after vacuum distillation and spin drying,6.3 kg of off-white solid was obtained, yield 95%, HPLC purity: 99.0%.

References:

CN114436951,2022,A Location in patent:Paragraph 0076-0080