Reacción #64975

Ecuación de reacción

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

Disolventes

water

dioxane

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaThe mixture is heated
2. 2
   Temperaturaunder reflux overnight
3. 3
   Temperaturacooled
4. 4
   Filtraciónthe salts are filtered off with suction
5. 5
   Lavadowashed with dioxane
6. 6
   ConcentraciónThe filtrate is concentrated
7. 7
   workup.ADDITIONK2CO3 is added
8. 8
   ExtracciónThe mixture is extracted with CHCl3
9. 9
   Secadothe extract is dried over K2CO3
10. 10
    Concentraciónconcentrated
11. 11
    workup.DISTILLATIONthe residue is distilled

Procedimiento

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.

Fuente