反应详情

3 mL acetic anhydride was added to 8.4 g benzyl 4-amino-5-hydroxy-azepane-1-carboxylic acid benzyl ester in 115 ml dichloromethane at 0° C. After 1 h at RT, saturated sodium bicarbonate was added. The phases were separated and the aqueous phase was extracted with dichloromethane. The combined organic phase was washed with brine, dried over sodium sulphate, filtered and concentrated. The residue was purified by chromatographie on silica gel (ethyl acetate/hexane 2:1) to yield 4.5 g of the desired product. (M+H)+: 307

1. customThe phases were separated
2. extractionthe aqueous phase was extracted with dichloromethane
3. washThe combined organic phase was washed with brine
4. dry with materialdried over sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by chromatographie on silica gel (ethyl acetate/hexane 2:1)