反应详情

A solution of benzyl N-allyl-N-[(2E)-2-hydroxyiminoethyl]carbamate (24 g, 96.6 mmol) in dichloromethane (338 mL) is treated drop wise over 10 minutes with a 5% w/w aqueous solution of sodium hypochlorite (106.08 mmol, 143.06 mL). The resultant mixture is stirred at room temperature overnight. The reaction is quenched with a 40% aqueous solution of sodium bisulfite (7 g). The organic layer is separated, dried over magnesium sulfate, and concentrated under vacuum. The crude product is purified over silica gel eluting with 5% ethyl acetate in hexanes to give the title compound (18 g, 75%). ES/MS (m/e): 247 (M+H).

1. customThe reaction is quenched with a 40% aqueous solution of sodium bisulfite (7 g)
2. customThe organic layer is separated
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated under vacuum
5. customThe crude product is purified over silica gel eluting with 5% ethyl acetate in hexanes