HRID29772

反应详情

EQUATION

反应方程式

HRID 29772 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

200 mg (0.58 mmol) of the product obtained in Example 1, in the form of the free amine, and 105 μl (0.81 mmol) of 2,5-dimethoxytetrahydrofuran are added to a two-phase mixture of 2.5 ml of water, 0.95 ml of AcOH and 2.85 ml of dichloro-1,2-ethane. The mixture is stirred at 80° C. for 2 hours, allowed to return to ambient temperature and extracted with CH2Cl2. The organic phase is washed with saturated aqueous NaCl solution and dried over MgSO4. The expected product is purified by chromatography on a silica column (CH2Cl2/heptane 75/25).

WORKUP

后处理

  1. customto return to ambient temperature
  2. extractionextracted with CH2Cl2
  3. washThe organic phase is washed with saturated aqueous NaCl solution
  4. dry with materialdried over MgSO4
  5. customThe expected product is purified by chromatography on a silica column (CH2Cl2/heptane 75/25)