反应 #2460282
ord-33455e0a8ae74f018e8007fa44191a18
反应方程式
反应条件
后处理
- 1其他A purple solution was formed which
- 2温度warmed to room temperature
- 3温度The reaction was heated in an oil-bath at 145° C. for 7 hours
- 4温度The reaction was then cooled to room temperature
- 5过滤This suspension was filtered
- 6其他the filtrate was evaporated to dryness
- 7其他a very clean reaction
- 8其他such for the next reaction
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.