HRID1357066

反应详情

EQUATION

反应方程式

HRID 1357066 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 1N 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)