Reacción #64963

Ecuación de reacción

water

N-methylhydroxylamine hydrochloride

sodium methylate

N-allyl-N-(1-oxoprop-2-yl)-urethane

→

methylhydroxylamine

Ethyl 2,8-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

Disolventes

methanol

toluene

toluene

Condiciones de reacción

Tratamiento posterior

1. 1
   Otrothe solution formed
2. 2
   Temperaturais heated
3. 3
   Temperaturaunder reflux
4. 4
   TemperaturaThe mixture is heated
5. 5
   Temperaturaunder reflux overnight
6. 6
   Extracciónthe product is extracted with dilute hydrochloric acid
7. 7
   Extracciónextracted with CHCl3
8. 8
   SecadoThe extract is dried over K2CO3
9. 9
   Concentraciónconcentrated
10. 10
    workup.DISTILLATIONthe residue is distilled

Procedimiento

A methanolic methylhydroxylamine solution is prepared from 16.4 g (0.2 mol) of N-methylhydroxylamine hydrochloride in 33 ml of absolute methanol and 36 g (0.2 mol) of 30% strength sodium methylate solution, and the solution formed is diluted with 130 ml of toluene and added dropwise to 354 g (0.17 mol) of N-allyl-N-(1-oxoprop-2-yl)-urethane in 250 ml of toluene, which is heated under reflux using a water separator. The mixture is heated under reflux overnight, the product is extracted with dilute hydrochloric acid and the hydrochloric acid solution is rendered alkaline with K2CO3 and extracted with CHCl3. The extract is dried over K2CO3 and concentrated and the residue is distilled.

Fuente