反应详情

To a suspension of sodium hydride (10 mg, 0.43 mmol) in dry THF (1 mL) was added 4-(2-amino-phenyl)-4-oxo-butyric acid ethyl ester (80 mg, 0.36 mmol) under Argon at −40° C. The reaction mixture was then allowed to warm up to rt over 3 h, and then added to water (20 mL). The mixture was then extracted with DCM (3×15 mL) and the combined extracts were then dried (sodium sulfate), and evaporated to leave an off-white solid. Recrystallization from EtOAc afforded a white solid (51 mg, 81%), m/z 175 (M).

1. extractionThe mixture was then extracted with DCM (3×15 mL)
2. dry with materialthe combined extracts were then dried (sodium sulfate)
3. customevaporated
4. customto leave an off-white solid
5. customRecrystallization from EtOAc