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
CONDITIONS
反应条件
- 温度
- 90 °C
PROCEDURE
实验过程
1-Benzoyl-2-(3-chlorophenyl)-2,3-dihydro-pyridin-4-one (910 mg) was placed in an argon filled flask together with 42 mg Pd(II) TFA2, 108 mg binaphthyl-di-tert-butyl phosphine, 39 mg zinc powder, 203.4 mg zinc cyanide and 45 ml dimethylacetamide. The solution was degassed with argon and heated at 90° C. for eight hours. After cooling to room temperature, the mixture was filtered through glass fiber filter paper. The supernatant was basified with ammonium hydroxide and the resulting mixture was extracted with diethyl ether. The combined ether extracts were dried over sodium sulfate, filtered, and concentrated in vacuo. Chromatography of the residue gave 350 mg 3-(1-benzoyl-4-oxo-1,2,3,4-tetrahydro-pyridin-2-yl)-benzonitrile.
WORKUP
后处理
- customThe solution was degassed with argon
- temperatureAfter cooling to room temperature
- filtrationthe mixture was filtered through glass fiber
- filtrationfilter paper
- extractionthe resulting mixture was extracted with diethyl ether
- dry with materialThe combined ether extracts were dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo