反应详情

In 470 ml of water were dissolved 60.2 g of β-piperidinopropiophenone hydrochloride and 18.1 g of hydroxylamine hydrochloride. To this solution was added portionwise 21.9 g of sodium hydrogencarbonate. After the whole amount was added, the mixture was stirred overnight. To the stirred mixture was then added an aqueous solution of 14.2 g of sodium hydroxide in 47 ml of water. Thus obtained mixture was well stirred and allowed to stand for 2 hours to produce a white precipitate. The precipitate was collected by filtration and washed successively with two portions of 200 ml of water and ethanol. The washed precipitate was dried to obtain a white solid. The solid was then recrystallized from methanol to obtain 41.2 g (yield: 74.8%) of the subject compound as a silver-white scaly product.

1. additionAfter the whole amount was added
2. stirringThus obtained mixture was well stirred
3. waitto stand for 2 hours
4. customto produce a white precipitate
5. filtrationThe precipitate was collected by filtration
6. washwashed successively with two portions of 200 ml of water and ethanol
7. customThe washed precipitate was dried
8. customto obtain a white solid
9. customThe solid was then recrystallized from methanol