反应详情

温度

30 °C

To a solution of 138b (1.0 g, 3.1 mmol) in methanol (35 mL) was added oxetan-3-one (669.6 mg, 9.3 mmol), NaBH3CN (585.9 mg, 9.3 mmol), and ZnCl2 (1.26 g, 9.3 mmol). The reaction was stirred at 30° C. for 2 h. The mixture was evaporated under reduced pressure and the residue diluted with water (20 mL). It was then extracted with dichloromethane (3×30 mL). The combined dichloromethane extract was concentrated under reduced pressure and the residue was purified by silica-gel column chromatography eluting with 40:1 ethyl acetate/methanol to afford 138c (291 mg, 25%) as a red solid. MS-ESI: [M+H]+ 376.3

1. customThe mixture was evaporated under reduced pressure
2. additionthe residue diluted with water (20 mL)
3. extractionIt was then extracted with dichloromethane (3×30 mL)
4. extractionThe combined dichloromethane extract
5. concentrationwas concentrated under reduced pressure
6. customthe residue was purified by silica-gel column chromatography
7. washeluting with 40:1 ethyl acetate/methanol