反应详情

Stir a mixture of 3.5 g (21.2 mmol) (2R)-1-(benzylamino)propan-2-ol [F. L. Delft, Synthesis 1997, 4, 450-454], 1.85 ml (2.0 g, 23.3 mmol) of a 35% aqueous formaldehyde solution and 3.6 ml (4.4 g, 95.3 mmol) formic acid for 16 h under reflux. After cooling to room temperature, first neutralize with 45% sodium hydroxide solution and then adjust to a pH value of 9. Extract with ethyl acetate. Wash the organic phase three times with 10 ml water each time, dry over sodium sulphate and filter. Concentrate the filtrate by vacuum evaporation, and dry. 3.08 g (78% of theor.) of the desired product is obtained.

1. temperatureunder reflux
2. extractionExtract with ethyl acetate
3. washWash the organic phase three times with 10 ml water each time
4. dry with materialdry over sodium sulphate
5. filtrationfilter
6. concentrationConcentrate the filtrate
7. customby vacuum evaporation
8. customdry