反応 #56269

反応方程式

carbamoyl chloride

phosgene

sym-dimethylurea

phosgene

→

N-Methylcarbamoyl-N-methylcarbamoyl chloride

溶媒

dichloroethane

dichloroethane

反応条件

後処理

1. 1
   workup.ADDITIONTo a cold suspension of 22 g
2. 2
   workup.STIRRINGto stir at room temperature for one hour
3. 3
   その他purged with nitrogen for one hour
4. 4
   その他The reaction mixture was evaporated under reduced pressure
5. 5
   抽出the residual gum was extracted twice with 350 ml
6. 6
   その他evaporated
7. 7
   その他to provide 25 g

実験手順

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.

出典