反应详情

温度

0 °C

A solution of 2-bromoanisole (50.0 g, 0.267 mol) in ether is added portionwise to a mixture of magnesium (7.10 g, 0.293 mol) in ether. After the addition is complete, the reaction mixture is heated at reflux for one hour, diluted with ether, cooled to 0° C., treated with a solution of 2-chloro-5-nitrobenzaldehyde (39.0 g, 0.210 mol) in tetrahydrofuran, warmed to room temperature, and diluted with an ice-water mixture. After acidifying the aqueous mixture with hydrochloric acid (pH 2-pH 3), the organic phase is separated and the aqueous phase is extracted with ether. The organic extracts are combined, washed sequentially with 10% sodium hydrogen carbonate solution and brine, dried over anhydrous sodium sulfate, and concentrated in vacuo to give the title product as a brown gum.

1. additionAfter the addition
2. temperaturethe reaction mixture is heated
3. temperatureat reflux for one hour
4. temperaturewarmed to room temperature
5. customthe organic phase is separated
6. extractionthe aqueous phase is extracted with ether
7. washwashed sequentially with 10% sodium hydrogen carbonate solution and brine
8. dry with materialdried over anhydrous sodium sulfate
9. concentrationconcentrated in vacuo