Réaction #64971

Équation de réaction

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

Solvants

water

dioxane

Conditions de réaction

Traitement

1. 1
   TempératureThe mixture is heated
2. 2
   Températureunder reflux overnight
3. 3
   Températurecooled
4. 4
   Filtrationthe salts are filtered off with suction
5. 5
   Lavagewashed with dioxane
6. 6
   ConcentrationThe filtrate is concentrated
7. 7
   workup.ADDITIONK2CO3 is added
8. 8
   ExtractionThe mixture is extracted with CHCl3
9. 9
   Séchagethe extract is dried over K2CO3
10. 10
    Concentrationconcentrated
11. 11
    workup.DISTILLATIONthe residue is distilled

Mode opératoire

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.

Source