HRID1596563

反应详情

EQUATION

反应方程式

HRID 1596563 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

3.57 g of mesitylacetyl chloride and 5.27 g of diisopropylethylamine were added at 0° C. to a solution of 5.0 g of (1b) in 50 ml of dioxane. The reaction mixture was stirred at 0° C. for 1 h, and was then allowed to warm to room temperature. The solution was added to water and acidified with 1 N HCl, extracted with dichloromethane, dried over MgSO4 and concentrated. Chromatographic purification on silica gel (dichloromethane/methanol 20:1) afforded a white solid (yield: 6.0 g).

WORKUP

后处理

  1. temperatureto warm to room temperature
  2. extractionextracted with dichloromethane
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. customChromatographic purification on silica gel (dichloromethane/methanol 20:1)