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