反应详情

A solution of (4-formylphenyl)carbamic acid tert-butyl ester (1.0 g), hydroxylamine hydrochloride (0.31 g), and sodium acetate (0.37 g) in ethanol (8.5 mL)/water(1.5 mL) is heated at reflux temperature for 1 hour. The mixture is cooled to ambient temperature and partitioned between diethyl ether and water. The aqueous layer is back-extracted with diethyl ether and the combined organic extracts are washed with saturated sodium chloride, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give 0.8 g pure white solid as the product. MS: m/z 237 (M+H)+.

1. temperatureat reflux temperature for 1 hour
2. custompartitioned between diethyl ether and water
3. extractionThe aqueous layer is back-extracted with diethyl ether
4. washthe combined organic extracts are washed with saturated sodium chloride
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure