反应详情

4-Hydroxymethyl-2,2,4-trimethyl-1,3-dioxolane (10g, prepared as in (b)) was added dropwise to a stirred suspension of sodium hydride (3g, 50% dispersion in oil) in dry toluene (150 ml). When the addition was complete the solution was heated under reflux until no more hydrogen was evolved. Benzyl chloride (7.85g) was added to the refluxing solution over a period of 15 minutes, after which the solution was heated under reflux for a further 3 hours. The solution was then cooled, washed with water (3 × 30 ml), dried and the solvent removed under reduced pressure. The residual oil was fractionally distilled to give the desired product as a colorless liquid having a b.p. 80° C at 0.2 mm Hg.

1. additionWhen the addition
2. temperaturewas heated
3. temperatureafter which the solution was heated
4. temperatureunder reflux for a further 3 hours
5. temperatureThe solution was then cooled
6. washwashed with water (3 × 30 ml)
7. customdried
8. customthe solvent removed under reduced pressure
9. distillationThe residual oil was fractionally distilled