反应详情

To hydroxylamine hydrochloride (15.86 g, 228.2 mmol) in H2O (35 mL) cooled in an ice-salt bath was added 7.1 N NaOH (27.4 mL, 194.4 mmol) followed by 1,4-dioxane (100 mL). The solution was vigorously stirred for 15 min and then chlorodiphenylphosphine oxide (20.00 g, 84.52 mmol) was added as a solution in 1,4-dioxane (100 mL). The solution was stirred an additional 15 min as a white precipitate formed which was filtered. The solid was suspended in 0.25 N NaOH (250 mL) while stirring in an ice-salt bath for 1 h. The solid was then collected, washed with H2O (100 mL), and thoroughly dried under vacuum to afford 7.09 g of the above compound as a white powder (30.4 mmol, yield 36%). 1H-NMR (DMSO-d6) δ 7.72 to 7.67 (m, 4H), 7.50 to 7.40 (m, 6H); −P-NMR (DMSO-d6) δ 23.11 (br s, 1P).

1. stirringThe solution was stirred an additional 15 min as a white precipitate
2. customformed which
3. filtrationwas filtered
4. stirringwhile stirring in an ice-salt bath for 1 h
5. customThe solid was then collected
6. washwashed with H2O (100 mL)
7. customthoroughly dried under vacuum