反应详情

A mixture of 104 g of glycerol formal, 152 g of methyl 5-norbornene-2-carboxylate, 2.0 g of sodium methoxide and 300 ml of toluene was heated under reflux for 5 hours while gradually distilling off methanol formed during the reaction. After cooling, the reaction solution was washed with saturated sodium bicarbonate water, dried over anhydrous sodium sulfate, and concentrated in vacuum. It was further purified by vacuum distillation, obtaining 209 g of a mixture of (1,3-dioxolan-4-yl)methyl 5-norbornene-2-carboxylate and 1,3-dioxan-5-yl 5-norbornene-2-carboxylate (boiling point 111-115° C./530 Pa, yield 93%).

1. temperaturewas heated
2. temperatureunder reflux for 5 hours
3. distillationwhile gradually distilling off methanol
4. customformed during the reaction
5. temperatureAfter cooling
6. washthe reaction solution was washed with saturated sodium bicarbonate water
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationconcentrated in vacuum
9. distillationIt was further purified by vacuum distillation