HRID2204924

反应详情

EQUATION

反应方程式

HRID 2204924 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureAfter 6 h the reaction mixture is cooled down to at least 30° C
  2. filtrationfilter off
  3. stirringstir for 30 min
  4. filtrationThe precipitate is filtered off
  5. washwashed with water
  6. customdried under vacuum at r40° C