反应详情

To a solution of the title compound of Step C (8.9 g) in methanol (120 mL)/water (50 mL) was added sodium acetate (7.5 g) followed by the addition of hydroxylamine hydrochloride (3.8 g). The mixture was heated at reflux overnight, cooled to room temperature, and concentrated to an oil. The oil was mixed with water and extracted three times with methylene chloride. The combined organic phases were dried (MgSO4), concentrated, and chromatographed on silica gel with 8% ethyl acetate/hexane to afford the title compound of Step D as an oil. 1H NMR (CDCl3): δ 8.8 (br s,1H), 7.77 (s,1H), 7.5 (m,2H), 7.37 (t,1H), 2.31 (s,3H), 0.27 (s,8H).

1. temperatureThe mixture was heated
2. temperatureat reflux overnight
3. concentrationconcentrated to an oil
4. additionThe oil was mixed with water
5. extractionextracted three times with methylene chloride
6. dry with materialThe combined organic phases were dried (MgSO4)
7. concentrationconcentrated
8. customchromatographed on silica gel with 8% ethyl acetate/hexane