HRID989582

反应详情

EQUATION

反应方程式

HRID 989582 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

Under nitrogen gas stream, a solution of 400 g (1510 mmol) of the crude 3-(trans-4-(trans-4-propylcyclohexyl)cyclohexyl)propanal obtained in the same manner as in the third step in Example 1 in 2.0 l of THF was added by drops to a mixture which was prepared by adding 43.0 g (1130 mmol) of lithium aluminum hydride to 400 ml of THF cooled down to a temperature lower than 5° C., while being maintained at the same temperature. After finishing of the adding, they were stirred at room temperature for 6 hours. This reaction mixture was gradually added to 500 ml of 2N aqueous sodium hydroxide solution and stirred at 50° C. for 30 minutes. The reaction mixture was filtered with Celite, the solvent was distilled off under a reduced pressure, and the residue was extracted with 2.0 l of ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was distilled off under a reduced pressure to obtain 341 g of a crude 3-(trans-4-(trans-4-propylcyclohexyl)cyclohexyl)propanol.

WORKUP

后处理

  1. additionwas added by drops to a mixture which
  2. customwas prepared
  3. temperaturewhile being maintained at the same temperature
  4. stirringstirred at 50° C. for 30 minutes
  5. filtrationThe reaction mixture was filtered with Celite
  6. distillationthe solvent was distilled off under a reduced pressure
  7. extractionthe residue was extracted with 2.0 l of ethyl acetate
  8. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  9. distillationthe solvent was distilled off under a reduced pressure