反应详情

A solution of 18.90 g (46.9 mmol) of 4-(4-bromophenoxy)-2,5-dimethylnitrobenzene in 150 ml of dioxane and 150 ml of hydrochloric acid is admixed with 31.77 g (140.8 mmol) of tin(II) chloride dihydrate at room temperature and the mixture is then refluxed for 3.5 h. It is cooled to room temperature, neutralized with 10% strength aqueous sodium hydroxide solution and extracted repeatedly with ethyl acetate, and the extracts are dried over Na2SO4 and filtered, and the solvent is removed under reduced pressure. This is followed by purification by column chromatography (8.10 g, purity 88.0%, yield 51.9%, log P (pH 2.3)=2.88).

1. temperaturethe mixture is then refluxed for 3.5 h
2. extractionextracted repeatedly with ethyl acetate
3. dry with materialthe extracts are dried over Na2SO4
4. filtrationfiltered
5. customthe solvent is removed under reduced pressure
6. customThis is followed by purification by column chromatography (8.10 g, purity 88.0%, yield 51.9%, log P (pH 2.3)=2.88)