HRID2357713
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
A mixture of 1-(4-chlorophenyl)pentane-1,4-dione (5.0 g., 0.024 mol, as obtained in Step-1) and 4-chloroaniline (3.33 g, 0.026 mol) in benzene (5.0 ml) was refluxed either over molecular sieves or using a Dean Stark apparatus. After three hours, benzene was removed under reduced pressure and the residue dissolved in ethyl acetate, washed with water (2×100 ml.) and brine (1×50 ml). The ethyl acetate layer was dried over anhydrous sodium sulfate, and the solvent evaporated off. The solid so obtained was washed with hexane to give 2.83 g (39.45%) of the title compound.
WORKUP
后处理
- temperaturewas refluxed either over molecular sieves
- custombenzene was removed under reduced pressure
- dissolutionthe residue dissolved in ethyl acetate
- washwashed with water (2×100 ml.) and brine (1×50 ml)
- dry with materialThe ethyl acetate layer was dried over anhydrous sodium sulfate
- customthe solvent evaporated off
- customThe solid so obtained
- washwas washed with hexane