反应详情

温度

0 °C

DAST (0.2 mL, 1.5 mmol) was added to N-[2-({(3R)-1-[4-hydroxy-4-(1,3-thiazol-2-yl)cyclohexyl]pyrrolidin-3-yl}amino)-2-oxoethyl]-3-(trifluoromethyl)benzamide (0.06 g, 0.12 mmol) in CH2Cl2 (5 mL) at −78° C. with stirring under N2. The solution was allowed to warm to 0° C. slowly and stirred for 1 h. Water and EtOAc were added. The aqueous layer was extracted with EtOAc (3×). The combined organic layers were washed with saturated NaCl, dried (MgSO4), concentrated and purified by flash chromatography and reverse-phase HPLC to give 0.020 g of the title compound in 31% yield. MS (EI) calcd: (M+H)+=499.2; found: 499.1.

1. stirringstirred for 1 h
2. extractionThe aqueous layer was extracted with EtOAc (3×)
3. washThe combined organic layers were washed with saturated NaCl
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. custompurified by flash chromatography and reverse-phase HPLC