反应详情

Hydroxylamine hydrochloride (52.6 g) was dissolved in water (150 ml) and stirred while an ice-cold solution of sodium hydroxide (30.28 g) in water (100 ml) was added. This solution was stirred for 15 minutes then absolute ethanol (600 ml) added and the solution stirred for a further 15 minutes. Ethyl ethoxymethyleneacetoacetate (128 g) was dissolved in absolute ethanol (100 ml) and added to the hydroxylamine solution. After stirring for 30 hours the solvents were removed on a rotary evaporator (bath at 45° C.). The clear oil was distilled at reduced pressure through a 15 cm Vigreux column. Product collected as a clear oil at 50°-54° C./0.5 mmHg.

1. additionwas added
2. stirringthe solution stirred for a further 15 minutes
3. stirringAfter stirring for 30 hours the solvents
4. customwere removed on a rotary evaporator (bath at 45° C.)
5. distillationThe clear oil was distilled at reduced pressure through a 15 cm Vigreux column
6. customProduct collected as a clear oil at 50°-54° C./0.5 mmHg