HRID1487237

反应详情

EQUATION

反应方程式

HRID 1487237 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of cesium carbonate (55.78 g, 171 mmol) in acetonitrile (500 mL) at room temperature was added N-methylmethane-sulfonamide (14.0 g, 0.128 mol). 2-Fluoro-benzonitrile (10.37 g, 86 mmol) was then added in portions over 10-15 minutes. The reaction mixture was stirred at room temperature for 12 hours. Upon completion, the mixture was filtered and then concentrated. The residue diluted with water and extracted by dichloromethane. The organic phases were combined, washed by brine, dried over anhydrous sodium sulfate and evaporated to afford the product N-(2-cyanophenyl)-N-methylmethane-sulfonamide (16.0 g, yield 88.9%). 1H NMR (400 MHz, CDCl3) δ ppm 7.62-7.73 (m, 2H), 7.54-7.56 (m, 1H), 7.45-7.50 (m, 1H), 3.40 (s, 3H), 3.14 (s, 3H).

WORKUP

后处理

  1. filtrationUpon completion, the mixture was filtered
  2. concentrationconcentrated
  3. additionThe residue diluted with water
  4. extractionextracted by dichloromethane
  5. washwashed by brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customevaporated