反应详情

1,1-Dimethylethyl 4-({4-[(trifluoromethyl)oxy]phenyl}sulfonyl)-1-piperazinecarboxylate (may be prepared as described in Intermediate 10; 5.450 g, 13.28 mmol) was dissolved in DCM (80 ml) and then 4M hydrochloric acid in dioxane (33.2 mL, 133 mmol) was added at room temperature and the reaction mixture was stirred for two hours. The reaction mixture was partitioned between DCM and aqueous sodium bicarbonate (30 ml). The organic phase was washed with further sodium bicarbonate (2×20 ml) and water (2×20 ml). The aqueous phase (pH 1) was basified by adding sodium hydroxide then the aqueous phase was extracted with DCM (2×20 ml). The solvent was removed under vacuum to give the title compound (3.5 g) as a white solid.

1. customThe reaction mixture was partitioned between DCM and aqueous sodium bicarbonate (30 ml)
2. washThe organic phase was washed with further sodium bicarbonate (2×20 ml) and water (2×20 ml)
3. additionby adding sodium hydroxide
4. extractionthe aqueous phase was extracted with DCM (2×20 ml)
5. customThe solvent was removed under vacuum