반응 #982265

반응 방정식

4-(trans-4-propylcyclohexyl)cyclohexanone

pyrrolidine

water

→

1-(4-(trans-4-propylcyclohexyl)-cyclohexen-1-yl)-pyrrolidine

용매

toluene

반응 조건

후처리

1. 1
   온도The solution was heated
2. 2
   기타is evaporated by azeotropic distillation
3. 3
   기타was removed
4. 4
   workup.DISTILLATIONAzeotropic distillation of the solution
5. 5
   기타was removed

실험 절차

200 g of 4-(trans-4-propylcyclohexyl)cyclohexanone and 135.2 g of pyrrolidine were dissolved in 800 ml of toluene. The solution was heated and stirred for 6 hours while water which is evaporated by azeotropic distillation was removed. Azeotropic distillation of the solution was carried out with toluene so that excessive pyrrolidine was removed, and 1-(4-(trans-4-propylcyclohexyl)-cyclohexen-1-yl)-pyrrolidine was obtained. The product as it was was cooled to room temperature, and 800 ml of toluene was added again. The mixture was cooled in a water bath, and 150 ml toluene solution of 89 ml of methyl vinyl ketone was added dropwise over a period of 2 hours at 20° C. or less. After the dropwise addition was completed, the temperature was increased over a period of 2 hours to reach the reflux temperature. The solution was cooled to room temperature, and a buffer solution of pH 5 which was prepared from B5.2 g of sodium acetate, 104.2 ml of acetic acid, and 104.2 ml of water was added. Reflux was further continued for 5 hours. After the solution was cooled to room temperature, the organic phase was separated and rinsed with water and a saturated saline solution. The organic phase was dried on anhydrous sodium sulfate. The solvent was evaporated, and 313 g of 6-(trans-4-propylcyclohexyl)-4,4a,5,6,7,8-hexahydro-2(3H)-naphthalenone was obtained.

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