反应详情

温度

80 °C

A stirred suspension of 2-acetamido-4-methyl-thiazole-5-sulfonic acid (2-dimethylamino-ethyl)-amide (1.0 g, 3.26 mmol) in 6N hydrochloric acid (13 ml) was heated for 2 h at 80° C., and 2N NaHCO3 solution (100 ml) was added. The mixture was extracted with ethyl acetate (3×50 ml), the combined organic layers washed with brine (50 ml) and dried (MgSO4). The crude product was further purified by crystallization (ethyl aceate) to yield the title compound (0.68 g, 79%) as a white solid. MS (ISP) 262.9 [(M−H)−]; mp 153° C.

1. extractionThe mixture was extracted with ethyl acetate (3×50 ml)
2. washthe combined organic layers washed with brine (50 ml)
3. dry with materialdried (MgSO4)
4. customThe crude product was further purified by crystallization (ethyl aceate)