反应详情

A solution of 3 g of 2',4'-dichloro-2-(3-pyridyl)-acetophenone oxime in 25 ml of dimethoxyethane is treated portionwise with 0.51 g of sodium hydride dispersion (55% in oil) and the mixture is stirred for 30 minutes at room temperature. Thereupon, 2.0 g of ethyl iodide are added and the mixture is heated at reflux temperature. After 4 hours, the mixture is poured onto ice and extracted with ethyl acetate. The organic phase is dried over sodium sulfate and concentrated under reduced pressure. The crude product is purified by chromatography on silica gel to yield 2',4'-dichloro-2-(3-pyridyl)-acetophenone O-ethyl oxime as a yellowish oil.

1. temperaturethe mixture is heated
2. temperatureat reflux temperature
3. waitAfter 4 hours
4. additionthe mixture is poured onto ice
5. extractionextracted with ethyl acetate
6. dry with materialThe organic phase is dried over sodium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe crude product is purified by chromatography on silica gel