HRID578874

反应详情

EQUATION

反应方程式

HRID 578874 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2 g of 2,6-dichloro-3-chloromethyl-pyridine in 8 ml of ethanol at ambient temperature was treated with 0.57 g of NaCN. The resulting brown suspension was refluxed for 2 h. Ethanol was removed by evaporation under reduced pressure and the residue was taken-up in water and ethyl acetate. The aqueous layer was washed twice with ethyl acetate. The organic phases were combined, dried over anhydrous sodium sulphate, filtered and concentrated. 2.05 g of crude 2,6-dichloro-pyridin-3-yl)-acetonitrile was obtained as brown solid which was used in the next step without further purification. 1H-NMR (CDCl3): 7.86 ppm (d, 1H), 7.38 ppm (d, 1H), 3.84 ppm (s, 2H).

WORKUP

后处理

  1. temperatureThe resulting brown suspension was refluxed for 2 h
  2. customEthanol was removed by evaporation under reduced pressure
  3. washThe aqueous layer was washed twice with ethyl acetate
  4. dry with materialdried over anhydrous sodium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. custom2.05 g of crude 2,6-dichloro-pyridin-3-yl)-acetonitrile was obtained as brown solid which
  8. customwas used in the next step without further purification