反应详情

温度

80 °C

A stirred suspension of 2-acetamido-4-methyl-thiazole-5-sulfonic acid (2-hydroxy-1-hydroxymethyl-ethyl)-amide (1.45 g, 4.69 mmol) in 6N hydrochloric acid (22 ml) was heated for 2 h at 80° C., evaporated, and saturated NaHCO3 solution (50 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 (0.55 g, 44%) as an off-white solid. MS (ISP) 266.0 [(M−H)−].

1. customevaporated
2. additionsaturated NaHCO3 solution (50 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)