反应详情

To a solution of 2-(hydroxymethyl)-1,3-propanediol (3.0 g) and dimethoxymethyl)benzene (6.36 ml) in DMF (50 ml) was added D-10-camphorsulfonic acid (1.31 g), and the mixture was stirred at ambient temperature overnight. To a reaction mixture were added triethylamine (1.18 ml) and water (150 ml) and the solution was extracted twice with ethyl acetate (150 ml). The extracts were washed with saturated aqueous sodium chloride, dried over magnesium sulfate and evaporated in vacuo. The resulting residue was chromatographed on silica gel (200 ml) eluting with a mixture of hexane and ethyl acetate (1:1 v/v). The fractions containing the object compound were collected and evaporated under reduced pressure to give (2-phenyl-1,3-dioxan-5-yl)methanol (4.51 g).

1. extractionthe solution was extracted twice with ethyl acetate (150 ml)
2. washThe extracts were washed with saturated aqueous sodium chloride
3. dry with materialdried over magnesium sulfate
4. customevaporated in vacuo
5. customThe resulting residue was chromatographed on silica gel (200 ml)
6. washeluting with a mixture of hexane and ethyl acetate (1:1 v/v)
7. additionThe fractions containing the object compound
8. customwere collected
9. customevaporated under reduced pressure