HRID333729

反应详情

EQUATION

反应方程式

HRID 333729 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A suspension of 5-hydroxy-1-methyl-3-(1-phenyl-1H-pyrazol-5-yl)pyridazin-4(1H)-one (201 mg), 1-(2-chloroethyl)-2,3-dihydro-1H-imidazo[1,2-a]benzimidazole (249 mg), cesium carbonate (428 mg) and sodium iodide (253 mg) in dimethylacetamide (10 mL) was stirred at 80° C. for 13 hr. The reaction mixture was filtered to separate an insoluble material, which was washed with ethyl acetate. The filtrate and washing were combined, and the mixture was concentrated under reduced pressure to dryness. The residue was purified by NH silica gel column chromatography (ethyl acetate/methanol) to give the title compound (227 mg) as a white solid.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. customto separate an insoluble material, which
  3. washwas washed with ethyl acetate
  4. washThe filtrate and washing
  5. concentrationthe mixture was concentrated under reduced pressure to dryness
  6. customThe residue was purified by NH silica gel column chromatography (ethyl acetate/methanol)