反应详情

温度

70 °C

To the stirred mixture of 25 g (0.29M) of 3-hydroxy-3-methyl-butyne, 50 ml of anhydrous N,N-dimethyl-formamide and 44.5 g (0.65M) imidazole cooled in an ice-bath was added 50 g (0.33M) tert.butyldimethylsilyl chloride. Stirring in the ice-bath was continued for 15 minutes and then at room temperate overnight. After addition of 250 mg of dimethylaminopyridine, the reaction mixture was heated at 70° C. for two hours and then poured into one liter of cold water. It was then extracted with 5×150 ml of ether. The organic extract was washed with brine, dried over MgSO4 and evaporated to dryness. The crude product was purified by vacuum distillation yielding 3-(tert.butyldimethylsilyl)oxy-3-methyl-butyne.

1. temperaturecooled in an ice-bath
2. customat room temperate overnight
3. extractionIt was then extracted with 5×150 ml of ether
4. extractionThe organic extract
5. washwas washed with brine
6. dry with materialdried over MgSO4
7. customevaporated to dryness
8. distillationThe crude product was purified by vacuum distillation