反应详情

50 mL of 1N hydrochloric acid is added dropwise to a solution of 10 g (30.88 mmol) of [(E)-2-(2-chloro-4-nitrophenyl)vinyl]dimethylamine in 200 mL of ethanol and the reaction mixture is then refluxed for 1 hour. Then the reaction mixture is evaporated down, diluted with water, and twice extracted with ethyl acetate. The combined organic phases are dried over sodium sulfate. The purification is carried out by column chromatography on silica gel (eluant: petroleum ether/ethyl acetate (3:1)). Yield: 4.5 g (73% of theory); C8H6ClNO3 (M=199.59); Rf value: 0.62 (silica gel, petroleum ether/ethyl acetate (1:1)).

1. temperaturethe reaction mixture is then refluxed for 1 hour
2. customThen the reaction mixture is evaporated down
3. additiondiluted with water
4. extractiontwice extracted with ethyl acetate
5. dry with materialThe combined organic phases are dried over sodium sulfate
6. customThe purification