HRID526170

反应详情

EQUATION

反应方程式

HRID 526170 的结构方程式

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

To a solution of tert-butyl trans-4-(dimethylamino)cyclohexylcarbamate (800 mg, 3.3 mmol) was added TFA (5 mL) and the reaction mixture was stirred with heat at 75° C. for 18 h. The reaction mixture was concentrated, the residue was loaded onto an SCX® ion-exchange column, flushed with methanol and then 7 N ammonia in methanol to obtain the desired product. The fractions containing the product were concentrated to dryness to obtain the desired product as the free base (400 mg, 85%) as an orange oil: ESI MS m/z 143 [C8H18N2+H]+.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. customflushed with methanol