Reaktion #64971

Reaktionsgleichung

sodium acetate

N-methylhydroxylamine hydrochloride

N-allyl-N-(2-oxopropyl)-acetamide

→

7-Acetyl-1,2-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane

Lösungsmittel

water

dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture is heated
2. 2
   Temperaturunder reflux overnight
3. 3
   Temperaturcooled
4. 4
   Filtrationthe salts are filtered off with suction
5. 5
   Waschenwashed with dioxane
6. 6
   EinengenThe filtrate is concentrated
7. 7
   workup.ADDITIONK2CO3 is added
8. 8
   ExtraktionThe mixture is extracted with CHCl3
9. 9
   Trocknenthe extract is dried over K2CO3
10. 10
    Einengenconcentrated
11. 11
    workup.DISTILLATIONthe residue is distilled

Vorschrift

15.5 g (0.1 mol) of N-allyl-N-(2-oxopropyl)-acetamide are dissolved in 100 ml of dioxane, and 9 g of anhydrous sodium acetate and 9 g (0. 108 mol) of N-methylhydroxylamine hydrochloride in 10 ml of water are added. The mixture is heated under reflux overnight and cooled and the salts are filtered off with suction and washed with dioxane. The filtrate is concentrated, the residue is taken up in 100 ml of water and K2CO3 is added. The mixture is extracted with CHCl3, the extract is dried over K2CO3 and concentrated and the residue is distilled.

Quelle