HRID1357005

反应详情

EQUATION

反应方程式

HRID 1357005 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3,5-dichloro-4-methyl-pyridine (13.86 g, 85.56 mmoles) in dry dimethylformamide (100 ml) was added, under nitrogen and stirring, with 55% NaH (3.73 g, 85.56 mmoles). The mixture was stirred for 1 hour then added with a solution of 5-cyclopentyloxy-1-chloro-6-methoxy-2H-phthalazine (7.95 g, 28.52 mmoles), obtained as described in example 7, in dry dimethylfomamide (70 ml). The mixture was left to stand for one night, quenched with water, diluted with water and extracted methyl aceate. The extract was washed with water and anhydrified over Na2SO4, then evaporated to dryness. The residue was flash chromatographed (eluent:petrolatum/ethyl acetate 1:1) to give 6.58 g of the title product (yield: 57%).

WORKUP

后处理

  1. customobtained
  2. waitThe mixture was left
  3. waitto stand for one night
  4. customquenched with water
  5. additiondiluted with water
  6. extractionextracted methyl aceate
  7. washThe extract was washed with water
  8. customevaporated to dryness
  9. customchromatographed (eluent:petrolatum/ethyl acetate 1:1)