HRID1846365
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
Anhydrous CuCl2 (0.370 g, 2.70 mmol) and 3,4-dinitrobenzaldehyde (0.270 g, 1.38 mmol) were added to a solution of 2-amino-N-(4-sec-butylphenyl)benzamide (0.370 g, 1.38 mmol) in anhydrous EtOH (20 mL). After heating to reflux temperature for 3 hours, the mixture was concentrated in vacuo. The residue was dissolved in EtOAc, washed with H2O, then brine, dried (Na2SO4), filtered, and concentrated in vacuo. Purification by flash chromatography on silica gel, eluting with 10% to 60% EtOAc in heptane, afforded 3-(4-sec-butylphenyl)-2-(3,4-dinitrophenyl)quinazolin-4(3H)-one (0.300 g, 49%).
WORKUP
后处理
- temperatureAfter heating
- temperatureto reflux temperature for 3 hours
- concentrationthe mixture was concentrated in vacuo
- dissolutionThe residue was dissolved in EtOAc
- washwashed with H2O
- dry with materialbrine, dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customPurification by flash chromatography on silica gel
- washeluting with 10% to 60% EtOAc in heptane