反应详情

A solution of ethyl magnesium bromide (70 ml, 1.3M in tetrahydrofuran) was stirred at 0°, under nitrogen. 2,2-Dimethyl-5-ethyl-5-formyl-1,3-dioxane (10.3 g.) in dry tetrahydrofuran (20 ml.) was added and the mixture was stirred at room temperature for three hours. The mixture was then refluxed, with stirring, for one hour. Saturated aqueous ammonium chloride solution was added to the cooled reaction mixture. The aqueous mixture was extracted with ether. The ether extracts were washed with water, dried over anhydrous magnesium sulphate and the solvent was removed in vacuo. The residue was purified by chromatography on silica gel, eluting with 40% ether hexane. 2,2-Dimethyl-5-ethyl-5-(1-hydroxy propyl)-1,3-dioxane was obtained as a colourless oil (10.0 g.).

1. temperatureThe mixture was then refluxed
2. stirringwith stirring, for one hour
3. extractionThe aqueous mixture was extracted with ether
4. washThe ether extracts were washed with water
5. dry with materialdried over anhydrous magnesium sulphate
6. customthe solvent was removed in vacuo
7. customThe residue was purified by chromatography on silica gel
8. washeluting with 40% ether hexane