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
- 80 °C
PROCEDURE
实验过程
15.44 g (140 mmol) of bromoethane and 8.95 g (59 mmol) of 2-(3,4-Dihydroxyphenyl)-acetonitrile are dissolved in 120 mL of N,N-dimethylformamide. 19.39 g (140 mmol) of potassium carbonate and 0.97 g (6 mmol) of potassium iodide are added to the mixture and the resulting suspension is heated to 80° C. After 6 h the reaction mixture is cooled down to at least 30° C. Pour the suspension on 200 mL of icy water, stir for ca. 20 min and filter off. Digest the solid in 120 mL of water, neutralize with hydrochloric acid 25% stir for 30 min. The precipitate is filtered off, washed with water and dried under vacuum at r40° C. 4.72 g of 2-(3,4-diethoxyphenyl)-acetonitrile are obtained as a white powder (39.3% yield). This material proves chromatographically homogenous and displays spectral characteristics consistent with its assigned structure.
WORKUP
后处理
- temperatureAfter 6 h the reaction mixture is cooled down to at least 30° C
- filtrationfilter off
- stirringstir for 30 min
- filtrationThe precipitate is filtered off
- washwashed with water
- customdried under vacuum at r40° C