HRID11199

反应详情

EQUATION

反应方程式

HRID 11199 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of isatin (2.5 g, 0.017 mol) in anhydrous DMF (50 ml) was cooled to 0° C. under a nitrogen atmosphere and treated with sodium hydride (0.5 g, 1.2 equivalents). A purple solution was formed which was stirred at 0° C. for 30 minutes and then warmed to room temperature. 4-Bromoanisole (2.13 ml, 1 equivalent) was added followed by copper iodide (6.46 g, 2 equivalents). The reaction was heated in an oil-bath at 145° C. for 7 hours. The reaction was then cooled to room temperature and diluted with an equal volume of ethyl acetate. This suspension was filtered and the filtrate was evaporated to dryness. TLC (1:4, ethyl acetate:hexanes) indicated a very clean reaction; Rf (product)=0.5. The crude material was used as such for the next reaction.

WORKUP

后处理

  1. customA purple solution was formed which
  2. temperaturewarmed to room temperature
  3. temperatureThe reaction was heated in an oil-bath at 145° C. for 7 hours
  4. temperatureThe reaction was then cooled to room temperature
  5. filtrationThis suspension was filtered
  6. customthe filtrate was evaporated to dryness
  7. customa very clean reaction
  8. customsuch for the next reaction