反应详情

To a solution of ethyl 1-(2-bromoacetyl)cyclopropanecarboxylate (4.7 g, 20 mmol) in THF (60 mL) was added (R)-α-methylbenzylamine (2.9 g, 24 mmol) and Et3N (4.04 g, 40 mmol). After stirring at rt for 3 days, the reaction mixture was concentrated in vacuo, and the residue was extracted with EtOAc (50 mL×2) and washed with water (30 mL). The combined organic phases were dried over anhydrous Na2SO4, filtered and the filtrate was concentrated in vacuo. The residue was purified by a silica gel column chromatography (EtOAc) to afford the title compound as a yellow solid (3.66 g, 80%).

1. concentrationthe reaction mixture was concentrated in vacuo
2. extractionthe residue was extracted with EtOAc (50 mL×2)
3. washwashed with water (30 mL)
4. dry with materialThe combined organic phases were dried over anhydrous Na2SO4
5. filtrationfiltered
6. concentrationthe filtrate was concentrated in vacuo
7. customThe residue was purified by a silica gel column chromatography (EtOAc)