反应详情

8-Ethoxycarbonyl-2-methyl-1-oxa-8-azaspiro [4.5 ]decan-3-one (20 g, 0.083 mol) was dissolved in absolute ethanol (1 L) and combined with triethylamine (11.5 ml) and hydroxylamine hydrochloride (5.7 g). The mixture was stirred at room temperature overnight. The ethanol was evaporated in vacuo and the residue was stirred with ether. The insoluble solids were filtered and the ether filtrate was evaporated. The residual oxime was purified by chomatography on silica gel and elution with ammoniated 2-10% MeOH/CHCl3. Evaporation of the solvents afforded the oxime, 11.5 g.

1. customThe ethanol was evaporated in vacuo
2. stirringthe residue was stirred with ether
3. filtrationThe insoluble solids were filtered
4. customthe ether filtrate was evaporated
5. customThe residual oxime was purified by chomatography on silica gel and elution with ammoniated 2-10% MeOH/CHCl3
6. customEvaporation of the solvents