反应详情

A solution of 3-ethenyl-6,7-dihydro[1,4]dioxino[2,3-c]pyridazine (11.58 g) in 1,4-dioxane/water (600 ml/180 ml), cooled in ice, was treated with an aqueous solution of osmium tetroxide (4% w/v, 25 ml) and sodium periodate (43 g). This mixture was allowed to warm to room temperature and after 7 hours under stirring the mixture was evaporated to dryness and azeotroped with 1,4-dioxane. Silica gel, 1,4-dioxane and chloroform were added and the mixture was evaporated to dryness overnight, then added to a silica column (400 g) and chromatographed, eluting with chloroform then 0-100% ethyl acetate in hexane, to afford a white solid (7.55 g, 64%).

1. customwas evaporated to dryness
2. customazeotroped with 1,4-dioxane
3. additionSilica gel, 1,4-dioxane and chloroform were added
4. customthe mixture was evaporated to dryness overnight
5. additionadded to a silica column (400 g)
6. customchromatographed
7. washeluting with chloroform