HRID1941042

反应详情

EQUATION

反应方程式

HRID 1941042 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Ethanol (20 ml) was added to the above 3-(4-(4-(2-(4-trifluoromethoxyphenyl)ethyl)cyclohexyl)cyclohexyl) propanal (2.70 g, 6.58 mmol), followed by cooling the mixture down to 0° C. in a nitrogen gas atmosphere, adding thereto, sodiumboronhydride (0.13 g, 3,43 mmol) so that the liquid temperature could not exceed 10° C., stirring the mixture at 0° C. for 2 hours, extracting the resulting product with ethyl acetate, washing the organic layer successively with a saturated aqueous solution of sodium bicarbonate and water, drying over magnesium sulfate, distilling off the solvent, and recrystallizing the residue from heptane, to obtain 3-(4-(4-(2-(4-trifluoromethoxyphenyl)ethyl)cyclohexyl)cyclohexyl)propanol (2.10 g, 5.09 mmol). Yield: 77.4%.

WORKUP

后处理

  1. additionadding
  2. customexceed 10° C.
  3. extractionextracting the resulting product with ethyl acetate
  4. washwashing the organic layer successively with a saturated aqueous solution of sodium bicarbonate and water
  5. dry with materialdrying over magnesium sulfate
  6. distillationdistilling off the solvent
  7. customrecrystallizing the residue from heptane