反应详情

温度

50 °C

A solution of 55.7 g (0.2 mol) of 3-methyl-1-(3-oxobutyl)-7-propylxanthine in a mixture of 200 ml each of dioxane and toluene was added dropwise in 45 minutes to a stirred suspension of 36.8 g (0.4 mol) of lithium acetylide as ethylenediamine complex and 98.6 g (0.4 mol) of anhydrous cerium(III) chloride in a mixture of 500 ml each of dry dioxane and toluene at 50° C. The mixture was then stirred at 50° C. for 7 hours, cooled and, after addition of cold water and acidification with 2 N hydrochloric acid, intensively extracted with chloroform, the extract was washed with water, dried over sodium sulfate and evaporated under reduced pressure, and the residue was purified by filtration through a silica gel column in the eluent chloroform/methanol (50:1), resulting in 35.0 g (58% of theory) of solid, which was recrystallized from ethanol with large losses.

1. temperaturecooled
2. extractionintensively extracted with chloroform
3. washthe extract was washed with water
4. dry with materialdried over sodium sulfate
5. customevaporated under reduced pressure
6. filtrationthe residue was purified by filtration through a silica gel column in the eluent chloroform/methanol (50:1)
7. customresulting in 35.0 g (58% of theory) of solid, which
8. customwas recrystallized from ethanol with large losses