反应详情

温度

80 °C

A stirred suspension of (RS)-1-(2-acetamido-4-methyl-thiazole-5-sulfonyl)-pyrrolidin-3-ol (0.82 g, 2.68 mmol) in 6N hydrochloric acid (13 ml) was heated for 2 h at 80° C. evaporated, and saturated NaHCO3 solution (20 ml) was added. The mixture was extracted with ethyl acetate (3×50 ml), the combined organic layers washed with brine (50 ml), dried (MgSO4) and evaporated. The crude product was further purified by crystallization (dichloromethane/MeOH/hexane) to yield the title compound (0.62 g, 88%) as a white solid. MS (ISP) 263.8 [(M+H)+]; mp 165° C.

1. customevaporated
2. additionsaturated NaHCO3 solution (20 ml) was added
3. extractionThe mixture was extracted with ethyl acetate (3×50 ml)
4. washthe combined organic layers washed with brine (50 ml)
5. dry with materialdried (MgSO4)
6. customevaporated
7. customThe crude product was further purified by crystallization (dichloromethane/MeOH/hexane)