反应详情

A mixture of 109d (500 mg, 1.3 mmol), and 30% formaldehyde (6.5 mmol) in methanol/HOAc (30 mL/3 mL) was stirred at room temperature for 5 minutes, followed by the addition of NaBH3CN (120 mg, 1.9 mmol). The mixture was stirred at room temperature for 4 h. It was cooled to room temperature and H2O (20 mL) was added. The mixture was extracted with DCM (50 mL) three times. The combined organic layer was concentrated under reduced pressure and the residue was purified by column chromatography eluting with 30:1 DCM/methanol to afford 109e as a yellow solid (473 mg, 83%). MS: [M+H]+ 392.

1. stirringThe mixture was stirred at room temperature for 4 h
2. temperatureIt was cooled to room temperature
3. extractionThe mixture was extracted with DCM (50 mL) three times
4. concentrationThe combined organic layer was concentrated under reduced pressure
5. customthe residue was purified by column chromatography
6. washeluting with 30:1 DCM/methanol