反应详情

温度

120 °C

To acetic anhydride (150 ml) (4SR,5RS)-(1-aza-bicyclo[3.3.1]nonan-4-ol (21.34 g, 151 mmol) is added portionwise under cooling. The reaction mixture is heated to 120° C. for 2.5 h, is evaporated and extracted with THF/sat. K2CO3 soln. The aq. layer is reextracted with THF. The combined organic layers are washed with brine, dried over Na2SO4, filtered and evaporated. The crude product is purified by bulb-to-bulb distillation (HV, 90° C.) to give 24.07 g (87%) of (4SR,5RS)-acetic acid 1-aza-bicyclo[3.3.1]non-4-yl ester.

1. temperatureunder cooling
2. customis evaporated
3. extractionextracted with THF/
4. washThe combined organic layers are washed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customevaporated
8. distillationThe crude product is purified by bulb-to-bulb distillation (HV, 90° C.)