HRID249474

反应详情

EQUATION

反应方程式

HRID 249474 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 40 ml of DMF was suspended 3.9 g (0.021 mole) of potassium phthalimide followed by addition of 3.9 g (0.02 mole) of 2,6-dichloro-3-pyridylmethyl chloride and the mixture was stirred at 60°-70° C. for 2 hours. The DMF was distilled off under reduced pressure and the residue was diluted with 50 ml of water and extracted with CHCl3 (50 ml×3). The extract was dried over MgSO4 and concentrated and the resulting precipitate was collected by filtration, washed with ether and dried to give 3.8 g of N-2,6-dichloro-3-pyridylmethyl)phthalimide as white prisms.

WORKUP

后处理

  1. distillationThe DMF was distilled off under reduced pressure
  2. additionthe residue was diluted with 50 ml of water
  3. extractionextracted with CHCl3 (50 ml×3)
  4. dry with materialThe extract was dried over MgSO4
  5. concentrationconcentrated
  6. filtrationthe resulting precipitate was collected by filtration
  7. washwashed with ether
  8. customdried