反应详情

5-Benzyloxymethyl-5-cyclohexyl-2,2-dimethyl-1,3-dioxane (3.0 g.) in dry ether (10 ml.) was added to liquid ammonia (100 ml.) at -70°. Sodium (0.5 g.) was added to the stirred solution. Stirring was maintained at -70°, for one hour. The mixture was then allowed to warm up to -30° and solid ammonium chloride (2.0 g.) was added. The ammonia was removed from the reaction mixture under a current of nitrogen. Water was added and the aqueous mixture was extracted with diethyl ether. The ethereal extracts were washed with water, dried over anhydrous magnesium sulphate and evaporated in vacuo. 5-Cyclohexyl-2,2-dimethyl-5-hydroxymethyl-1,3-dioxane was obtained as a cream solid (2.15 g.) and was used without further purification.

1. temperaturewas maintained at -70°, for one hour
2. temperatureto warm up to -30°
3. customThe ammonia was removed from the reaction mixture under a current of nitrogen
4. additionWater was added
5. extractionthe aqueous mixture was extracted with diethyl ether
6. washThe ethereal extracts were washed with water
7. dry with materialdried over anhydrous magnesium sulphate
8. customevaporated in vacuo