HRID1846371
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
Zn dust (2.0 g, 30.0 mmol) was added to a solution of (E)-3-(4-bromophenyl)-2-(3-(2-(dimethylamino)vinyl)-4-nitrophenyl)quinazolin-4(3H)-one (1.5 g, 3.0 mmol) in AcOH (25 mL). The mixture was stirred at room temperature overnight, then heated to reflux temperature for 1 hour. After cooling to 0° C., the reaction mixture was basified with 1 N NaOH and extracted with EtOAc. The organics were washed with brine, dried (Na2SO4), filtered, and concentrated in vacuo. Purification by flash chromatography on silica gel, eluting with 0% to 40% EtOAc in CH2Cl2, afforded 3-(4-bromophenyl)-2-(1H-indol-5-yl)quinazolin-4(3H)-one (0.225 g, 18%).
WORKUP
后处理
- temperatureheated
- temperatureto reflux temperature for 1 hour
- temperatureAfter cooling to 0° C.
- extractionextracted with EtOAc
- washThe organics were washed with brine
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customPurification by flash chromatography on silica gel
- washeluting with 0% to 40% EtOAc in CH2Cl2