HRID1766823

反应详情

EQUATION

反应方程式

HRID 1766823 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

To a solution of 3,3-dimethyl-1,2-epoxybutane (5.0 mL, 41.0 mmol) in DMF (100 mL) was added N-hydroxyphthalimide (8.03 g, 49.2 mmol) and triethylamine (6.90 mL, 49.2 mmol). The solution was heated at 75° C. for two days. The solution was cooled to room temperature, diluted with ethyl acetate and washed with water (2×), saturated potassium carbonate (3×), brine (2×), dried over Na2SO4 and concentrated to an orange solid. Purification using flash column chromatography (dichloromethane) provided the desired product as a white solid (1.50 g, 14%).

WORKUP

后处理

  1. temperatureThe solution was cooled to room temperature
  2. washwashed with water (2×), saturated potassium carbonate (3×), brine (2×)
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated to an orange solid
  5. customPurification