Reaktion #63290

Reaktionsgleichung

sodium hydrogencarbonate

β-piperidinopropiophenone hydrochloride

hydroxylamine hydrochloride

sodium hydroxide

→

subject compound

Ausbeute 74.8%

β-piperidinopropiophenone oxime

Ausbeute 74.8%

Lösungsmittel

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONAfter the whole amount was added
2. 2
   workup.STIRRINGThus obtained mixture was well stirred
3. 3
   workup.WAITto stand for 2 hours
4. 4
   Sonstigeto produce a white precipitate
5. 5
   FiltrationThe precipitate was collected by filtration
6. 6
   Waschenwashed successively with two portions of 200 ml of water and ethanol
7. 7
   SonstigeThe washed precipitate was dried
8. 8
   Sonstigeto obtain a white solid
9. 9
   SonstigeThe solid was then recrystallized from methanol

Vorschrift

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.

Quelle