HRID1846362
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
3-methyl-4-nitro-benzaldehyde (0.268 g, 1.60 mmol) and anyhydrous CuCl2 (0.437 g, 3.20 mmol) were added to a solution of 2-amino-N-(4-chlorophenyl)benzamide (0.400 g, 1.60 mmol) in anyhydrous EtOH (15 mL) and heated at reflux temperature for 3.5 hours. After concentration in vacuo and dissolving the residue in EtOAc, the organics were washed with H2O, then brine, dried (Na2SO4), filtered, and concentrated in vacuo. Purification by flash chromatography on silica gel, eluting with 10% to 70% EtOAc in heptane, afforded 3-(4-chlorophenyl)-2-(3-methyl-4-nitrophenyl)quinazolin-4(3H)-one (0.300 g, 48%).
WORKUP
后处理
- temperatureheated
- temperatureat reflux temperature for 3.5 hours
- concentrationAfter concentration in vacuo
- dissolutiondissolving the residue in EtOAc
- washthe organics were washed with H2O
- dry with materialbrine, dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customPurification by flash chromatography on silica gel
- washeluting with 10% to 70% EtOAc in heptane