HRID1381982

反应详情

EQUATION

反应方程式

HRID 1381982 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3 g (0.017 mol) of 2-chloroisonicotinoyl chloride was added dropwise to a solution of 2.8 g (0.02 mol) of 2-amino-2-(2-thienyl)acetonitrile and 1.6 g (0.02 mol) of pyridine in 30 ml of toluene while the temperature was kept at 10° to 15° C. The mixture was stirred at room temperature for 1 h. A saturated aqueous common salt solution was added thereto. The organic layer was separated and dried over anhydrous sodium sulfate. The solvent was concentrated under reduced pressure and the crude product was purified according to silica gel column chromatography to obtain 1.5 g (yield: 31.8%) of light brown crystals having a melting point of 123° to 125° C.

WORKUP

后处理

  1. customwas kept at 10° to 15° C
  2. additionA saturated aqueous common salt solution was added
  3. customThe organic layer was separated
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationThe solvent was concentrated under reduced pressure
  6. customthe crude product was purified
  7. customto obtain 1.5 g (yield: 31.8%) of light brown crystals