反应详情

To a stirred solution of N,N-dimethylethylenediamine (1.04 g, 11.8 mmol) in tetrahydrofurane (14 ml) was added at 0° C. (ice water bath) commercially available 2-acetamido-4-methylthiazole-5-sulfonyl chloride (1.0 g, 3.93 mmol) and triethylamine (0.6 ml, 4 mmol). The light yellow suspension was stirred at room temperature for 17 h, and evaporated. The crude product was further purified by column chromatography on silica gel (dichloromethane/MeOH/NH4OH 80:10:1) and subsequent crystallization (dichloromethane/hexane) to yield 2-acetamido-4-methyl-thiazole-5-sulfonic acid (2-dimethylamino-ethyl)-amide (1.07 g, 89%) as a white solid. MS (ISP) 305.1 [(M−H)−]; mp 143° C.

1. customevaporated
2. customThe crude product was further purified by column chromatography on silica gel (dichloromethane/MeOH/NH4OH 80:10:1) and subsequent crystallization (dichloromethane/hexane)