HRID2051584
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
N-phenyl-N'-(1,3-dimethylbutyl)-p-phenylenediamine (26.8g, 0.10 mol) in 100 mL chloroform and 30g (0.22 mol) of K2CO3 as a saturated aqueous solution are placed in a 250 mL, 3-neck round bottom flask. Thiophosgene (11.5g: 0.10 mol) in 20 mL chloroform is added at such a rate sufficient to reach and maintain reflux conditions. Stirring is continued until the mixture returns to room temperature. Methanol (6.4g, 0.2 mol) is then added and the mixture refluxed for 4 hours. The organic layer is separated, dried with MgSO4 and the solvent removed on a rotary evaporator to give the desired product.
WORKUP
后处理
- temperaturemaintain
- temperaturereflux conditions
- customreturns to room temperature
- temperaturethe mixture refluxed for 4 hours
- customThe organic layer is separated
- dry with materialdried with MgSO4
- customthe solvent removed on a rotary evaporator