반응 #56269

반응 방정식

carbamoyl chloride

phosgene

sym-dimethylurea

phosgene

→

N-Methylcarbamoyl-N-methylcarbamoyl chloride

용매

dichloroethane

dichloroethane

반응 조건

후처리

1. 1
   workup.ADDITIONTo a cold suspension of 22 g
2. 2
   workup.STIRRINGto stir at room temperature for one hour
3. 3
   기타purged with nitrogen for one hour
4. 4
   기타The reaction mixture was evaporated under reduced pressure
5. 5
   추출the residual gum was extracted twice with 350 ml
6. 6
   기타evaporated
7. 7
   기타to provide 25 g

실험 절차

To a cold suspension of 22 g. (0.25 m.) of sym-dimethylurea in dichloroethane was added dropwise with stirring a cold solution of 30 g. (0.3 m.) of phosgene in 90 ml. of dichloroethane. After the addition of the phosgene solution was complete, the reaction mixture was allowed to stir at room temperature for one hour and was then heated to 80° C. and purged with nitrogen for one hour. The reaction mixture was evaporated under reduced pressure and the residual gum was extracted twice with 350 ml. portions of either. The extracts were combined and evaporated to provide 25 g. of the carbamoyl chloride.

출처