HRID1856754
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of triphosgene (4.35 g) in toluene (70 ml) is added dropwise N-methylcyclohexylamine (5 g). To the mixture is added dropwise pyridine (3.5 g), and the mixture is refluxed for 4 hours. The mixture is allowed to cool, and the organic layer is separated, washed with 0.1 N hydrochloric acid, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to remove the solvent to give N-methyl-N-cyclohexylaminocarbonyl chloride (7.62 g) as a colorless oil.
WORKUP
后处理
- temperaturethe mixture is refluxed for 4 hours
- temperatureto cool
- customthe organic layer is separated
- washwashed with 0.1 N hydrochloric acid
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customto remove the solvent