反应详情

LiAlH4 (3.5 g, 74 mmol) was added over 2 hours to a cooled solution (0° C.) of 1-adamantylphosphonic acid dichloride (15 g, 59 mmol) in THF (250 cm3). The reaction was then allowed to warm to ambient temperature and was stirred for 20 hours. The grey suspension was then cooled (0° C.) and HCl (75 cm3, 1M) was slowly added via syringe, to afford a two phase system with some solid present in the lower phase. Concentrated HCl (8 cm3, 11M) was then added to improve the separation of the two layers. The (upper) THF phase was removed via cannula and dried over magnesium sulphate. After filtration via cannula, the volatiles were removed in-vacuo to afford the product.

1. additionwas slowly added via syringe
2. customto afford a two phase system with some solid present in the lower phase
3. customthe separation of the two layers
4. customThe (upper) THF phase was removed via cannula
5. dry with materialdried over magnesium sulphate
6. filtrationAfter filtration via cannula
7. customthe volatiles were removed in-vacuo
8. customto afford the product