반응 #81784

반응 방정식

1,2,3,4,4a,9a-hexahydrocarbazole

3-chloropropionyl chloride

→

9-(3-chloropropionyl)-1,2,3,4,4a,9a-hexahydrocarbazole

수율 111.7%

용매

acetone

acetone

반응 조건

후처리

1. 1
   온도the mixture was refluxed for 1 hour
2. 2
   workup.DISTILLATIONThe solvent was then distilled off under reduced pressure
3. 3
   workup.DISSOLUTIONthe residue was dissolved in 100 ml of dichloromethane
4. 4
   세척washed with 10% hydrochloric acid twice
5. 5
   건조The solution was dried over anhydrous sodium sulfate
6. 6
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure

실험 절차

To a solution of 10 g 1,2,3,4,4a,9a-hexahydrocarbazole in 30 ml acetone was added a solution of 8.3 g 3-chloropropionyl chloride in 30 ml acetone dropwise at ambient temperature and the mixture was refluxed for 1 hour. The solvent was then distilled off under reduced pressure and the residue was dissolved in 100 ml of dichloromethane and washed with 10% hydrochloric acid twice. The solution was dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure to provide about 17 g of 9-(3-chloropropionyl)-1,2,3,4,4a,9a-hexahydrocarbazole as a viscous oil. This oil was not purified but submitted directly to the next reaction.

출처