反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionwas added by drops to a mixture which
- customwas prepared
- temperaturewhile being maintained at the same temperature
- stirringstirred at 50° C. for 30 minutes
- filtrationThe reaction mixture was filtered with Celite
- distillationthe solvent was distilled off under a reduced pressure
- extractionthe residue was extracted with 2.0 l of ethyl acetate
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- distillationthe solvent was distilled off under a reduced pressure