HRID431998
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 solution of 4-(3-cyanophenyl)-1-trityl-1H-imidazole (0.07 g, 0.17 mmol) in tetrahydrofuran (1.36 mL) was treated with 2N hydrochloric acid (0.68 mL) and the resulting mixture was heated at reflux for 45 minutes. After cooling the reaction mixture was concentrated in vacuo and the residue dissolved in dichloromethane (20 mL). The organic phase was successively washed with 1N sodium hydroxide (10 mL), water (20 mL) and brine (20 mL). The organic solution was dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo. Silica gel chromatography of the residues using 3% methanol in dichloromethane afforded 0.02 g (72%) of 4-(3-cyanophenyl)imidazole as a white solid.
WORKUP
后处理
- temperaturethe resulting mixture was heated
- temperatureat reflux for 45 minutes
- temperatureAfter cooling the reaction mixture
- concentrationwas concentrated in vacuo
- dissolutionthe residue dissolved in dichloromethane (20 mL)
- washThe organic phase was successively washed with 1N sodium hydroxide (10 mL), water (20 mL) and brine (20 mL)
- dry with materialThe organic solution was dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo