HRID565226

反应详情

EQUATION

反应方程式

HRID 565226 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of 4,4-diphenylcyclohexanone (2.5 g) and ethylenediamine (10 g) and p-toluenesulfonic acid (100 mg) in benzene (200 mL) was refluxed for 4 h in Dean-Stark trap to remove the water that formed. Solvent was evaporated and the residue was redissolved in methanol (60 mL) and cooled to 0° C. To this, sodium borohydride (2 g) was added in portions and the mixture was stirred at room temperature for 3 h. Solvent was evaporated, the residue was dissolved in dichloromethane (300 mL), washed with brine (3×500 mL), dried (potassium carbonate), and the solvent evaporated to leave the product as a colorless viscous oil (2.94 g, 100%). The 1H-NMR showed this product to be pure and was used in the next step without any further purification.

WORKUP

后处理

  1. temperaturewas refluxed for 4 h in Dean-Stark trap
  2. customto remove the water
  3. customthat formed
  4. customSolvent was evaporated
  5. dissolutionthe residue was redissolved in methanol (60 mL)
  6. additionTo this, sodium borohydride (2 g) was added in portions
  7. customSolvent was evaporated
  8. dissolutionthe residue was dissolved in dichloromethane (300 mL)
  9. washwashed with brine (3×500 mL)
  10. dry with materialdried (potassium carbonate)
  11. customthe solvent evaporated