反应详情

A solution of 3-bromo-2-tert-butylsulfanyl-5-nitro-benzaldehyde (1.2 g, 3.8 mmol) and hydroxylamine hydrochloride (1.2 g, 7.7 mmol) in isopropanol (36 mL) and water (8 mL) was heated to 90° C. for 16 h. The reaction mixture was cooled and concentrated to remove isopropanol. Water was added to the residue, followed by saturated sodium bicarbonate solution until the pH was ˜8.0. The residue was extracted with dichloromethane (2×30 mL). The combined organic fractions were dried with sodium sulfate, filtered, and concentrated to afford 1.9 g of the crude title compound which was used without further purification.

1. temperatureThe reaction mixture was cooled
2. concentrationconcentrated
3. customto remove isopropanol
4. additionWater was added to the residue
5. extractionThe residue was extracted with dichloromethane (2×30 mL)
6. dry with materialThe combined organic fractions were dried with sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated