반응 #64975

반응 방정식

sodium acetate

N-methylhydroxylamine hydrochloride

ethyl N-(but-2-enyl)-N-(2-oxoethyl)-carbamate

→

Ethyl 2,4-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

용매

water

dioxane

반응 조건

후처리

1. 1
   온도The mixture is heated
2. 2
   온도under reflux overnight
3. 3
   온도cooled
4. 4
   여과the salts are filtered off with suction
5. 5
   세척washed with dioxane
6. 6
   농축The filtrate is concentrated
7. 7
   workup.ADDITIONK2CO3 is added
8. 8
   추출The mixture is extracted with CHCl3
9. 9
   건조the extract is dried over K2CO3
10. 10
    농축concentrated
11. 11
    workup.DISTILLATIONthe residue is distilled

실험 절차

18.4 g (0.1 mol) of ethyl N-(but-2-enyl)-N-(2-oxoethyl)-carbamate 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.

출처