HRID657620

反应详情

EQUATION

反应方程式

HRID 657620 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-(4-hydroxyphenyl)cyclohexanone (3 g) in tetrahydrofuran (20 mL) and a solution of methylamine in tetrahydrofuran (7.9 mL, 2 M) is stirred overnight at room temperature, concentrated under reduced pressure, dissolved in a mixture of dichloromethane and methanol (30 mL, 1/1) and cooled at a temperature close to 0° C. Sodium borohydride (822 mg) is added portionwise and the mixture is stirred at room temperature for one hour. The precipitate is filtered and washed with diethyl oxide to give 1.1 g of trans-4-(4-hydroxyphenyl)-N-methylcyclohexanamine used without further purification.

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. dissolutiondissolved in a mixture of dichloromethane and methanol (30 mL, 1/1)
  3. temperaturecooled at a temperature
  4. customclose to 0° C
  5. additionSodium borohydride (822 mg) is added portionwise
  6. filtrationThe precipitate is filtered
  7. washwashed with diethyl oxide