Phosgene → 2,4-Dimethylallophanoyl chloride
反応式
[CH3:1][NH:2][C:3]([NH:5][CH3:6])=[O:4].[C:7]([Cl:10])(Cl)=[O:8].C(Cl)(=O)N>ClC(Cl)C>[CH3:1][NH:2][C:3]([N:5]([CH3:6])[C:7]([Cl:10])=[O:8])=[O:4]参加物
5
反応条件
- 温度
- 80 °C
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.
後処理
- additionTo a cold suspension of 22 g
- stirringto stir at room temperature for one hour
- custompurged with nitrogen for one hour
- customThe reaction mixture was evaporated under reduced pressure
- extractionthe residual gum was extracted twice with 350 ml
- customevaporated
- customto provide 25 g
出典と根拠
- ORDレコード
- ord-9a365a89e9434375b38eca979ec4bea6
- 出典データセット
- uspto-grants-1980_09
- 特許番号
- US04224442
反応ノート
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