反应详情

2,2-Dimethyl-1,3-dioxane-4,6-dione (1.72 g) was suspended in anhydrous pyridine (20 ml) and cooled to 0° C. (2-methoxyethoxy)acetyl chloride (2 g) was added slowly. The mixture was stirred at room temperature for 3 h. The mixture was poured into 2 N HCl (30 ml) and extracted with DCM (×3). The combined organic phase was washed with water, brine, dried over sodium sulfate and concentrated in vacuo. The orange oil was dissolved in EtOH (20 ml) and was refluxed for 7 h. The solvent was removed in vacuo and the brown oil was Kugelrohr distilled affording the title compound as a colourless oil (1.55 g).

1. additionwas added slowly
2. extractionextracted with DCM (×3)
3. washThe combined organic phase was washed with water, brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo
6. dissolutionThe orange oil was dissolved in EtOH (20 ml)
7. temperaturewas refluxed for 7 h
8. customThe solvent was removed in vacuo
9. distillationdistilled