HRID1258054

反应详情

EQUATION

反应方程式

HRID 1258054 的结构方程式

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of thiophene-3-acetonitrile (6.15 g, 50 mmol) and MeI (12.5 mL, 4 equiv) in DMF (200 mL) was added sodium hydride (6 g, 60%, 3 equiv) at 0° C. under nitrogen and the reaction mixture was stirred for 3 h at 0° C. It was then quenched with water and extracted with hexane (3×100 mL). The combined organic layer was washed with water and dried over MgSO4. Evaporation of solvent afforded 2-methyl-2-thiophen-3-yl-propionitrile as an oil, which was used in next step without further purification. 1H-NMR(CDCl3): δ 8.02 (1H, m), 7.35 (1H, dd), 7.12 (1H, dd), 2.96 (3H, s), 2.89 (3H, s).

WORKUP

后处理

  1. customIt was then quenched with water
  2. extractionextracted with hexane (3×100 mL)
  3. washThe combined organic layer was washed with water
  4. dry with materialdried over MgSO4
  5. customEvaporation of solvent