反应详情

A solution of (4R-trans)-(-)-2,2-dimethyl-1,3-dioxolane-4,5-dimethanol (51 g) in THF (400 ml) was added dropwise to a stirred suspension of sodium hydride (17.5 g of 80% in oil) in THF (200 ml). After 0.75 h, benzyl bromide (116.3 g) was added dropwise and the resulting mixture was stirred for 18 h, and was then heated at reflux for 2 h. After stirring for a further 20 h at 20°, the mixture was cooled in ice, water (10 ml) was added and the mixture was evaporated to dryness. The residue was extracted with ER, and the organic solution was dried and the solvent was evaporated giving a crude product (130 g) which was used without further purification.

1. temperaturewas then heated
2. temperatureat reflux for 2 h
3. stirringAfter stirring for a further 20 h at 20°
4. temperaturethe mixture was cooled in ice
5. customthe mixture was evaporated to dryness
6. extractionThe residue was extracted with ER
7. customthe organic solution was dried
8. customthe solvent was evaporated