反应详情

25 g (144.5 mmol) of 3-bromophenol are placed in the presence of K2CO3 (21 g, 152 mmol) in 75 ml of ethyl 2-bromoisobutyrate and heated to reflux for 7 h. After elimination of K2CO3 by filtration, the reaction medium is dry concentrated. After purification by flash chromatography on silica (petroleum ether:AcOEt 90:10), 37 g of intermediate 10d are collected in the form of clear oil (yield=89%). TLC silica gel 60 F 254 Merck, petroleum ether:AcOEt 90:10, Rf=0.40.

1. temperatureheated
2. temperatureto reflux for 7 h
3. filtrationAfter elimination of K2CO3 by filtration
4. customthe reaction medium is dry
5. concentrationconcentrated
6. customAfter purification by flash chromatography on silica (petroleum ether:AcOEt 90:10), 37 g of intermediate 10d