反应详情

A solution of 2-[(3,6-dichloro-4-pyridazinyl)oxy]ethanol containing some bromo-derivative (15.46 g; 0.0703 mol) in dry 1,4-dioxane (1.2 L) was treated with lithium hydride (2.3 g; 0.28 mol) in portions and stirred at room temperature for 1 hour under argon, then heated at 110° C. overnight. The reaction mixture was quenched with wet 1,4-dioxane, then iced-water. The solution was evaporated to half volume, taken to pH 8 with 5M hydrochloric acid and evaporated to dryness. Water was added and the residue was extracted 5× with chloroform, dried (sodium sulphate) and evaporated to afford a white solid (12.4 g, ca. 77%) (containing ca. 15% of a bromo species).

1. temperatureheated at 110° C. overnight
2. customThe reaction mixture was quenched with wet 1,4-dioxane
3. customThe solution was evaporated to half volume
4. customevaporated to dryness
5. additionWater was added
6. extractionthe residue was extracted 5× with chloroform
7. dry with materialdried (sodium sulphate)
8. customevaporated
9. customto afford