반응 #640614

반응 방정식

1-aza-bicyclo[3.3.1]nonan-4-ol

acetic anhydride

→

(4SR,5RS)-acetic acid 1-aza-bicyclo[3.3.1]non-4-yl ester

수율 87.0%

반응 조건

후처리

1. 1
   온도under cooling
2. 2
   기타is evaporated
3. 3
   추출extracted with THF/
4. 4
   세척The combined organic layers are washed with brine
5. 5
   건조dried over Na2SO4
6. 6
   여과filtered
7. 7
   기타evaporated
8. 8
   workup.DISTILLATIONThe crude product is purified by bulb-to-bulb distillation (HV, 90° C.)

실험 절차

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 reextiacted 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.

출처