Reacción #64959

Ecuación de reacción

water

sodium methylate

N-methylhydroxylamine hydrochloride

N-(2-methyl-prop-2-enyl)-N-(2-oxoethyl)-urethane

→

Ethyl 2,5-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

Disolventes

toluene

methanol

Condiciones de reacción

Tratamiento posterior

1. 1
   FiltraciónThe sodium chloride is filtered off with suction
2. 2
   Lavadowashed with 8 ml of methanol and 80 ml of toluene
3. 3
   Temperaturais heated
4. 4
   TemperaturaThe mixture is heated
5. 5
   Temperaturaunder reflux overnight
6. 6
   Extracciónthe product is extracted with 160 ml of 10% strength hydrochloric acid
7. 7
   Extracciónextracted with six portions, of 200 ml of CHCl3
8. 8
   SecadoThe extracts are dried over K2CO3
9. 9
   Concentraciónconcentrated
10. 10
    workup.DISTILLATIONthe residue is distilled

Procedimiento

21.7 g of 30% strength sodium methylate solution are added dropwise to 10 g (0.12 mol) of N-methylhydroxylamine hydrochloride in 26 ml of methanol. The sodium chloride is filtered off with suction and washed with 8 ml of methanol and 80 ml of toluene. This solution is added dropwise to 19.2 g (0.11 mol) of N-(2-methyl-prop-2-enyl)-N-(2-oxoethyl)-urethane, which is heated under reflux in 160 ml of toluene using a water separator. The mixture is heated under reflux overnight, the product is extracted with 160 ml of 10% strength hydrochloric acid and the hydrochloric acid solution is rendered alkaline with potassium carbonate and extracted with six portions, of 200 ml of CHCl3. The extracts are dried over K2CO3 and concentrated and the residue is distilled.

Fuente