反应详情

Triethylamine (10.5 ml, 75 mmol) was added slowly to a solution of triphosgene (3.0 g, 10 mmol) and 2-hydroxypyridine (5.7 g, 60 mmol) in dry DCM (500 ml) at 0° C. under argon. The mixture was allowed to warm to room temperature and was stirred overnight. The solvent was removed under reduced pressure and the residue taken up in ethyl acetate (500 ml), washed with saturated aqueous sodium hydrogen carbonate (2×150 ml) and brine (200 ml), dried over anhydrous sodium sulphate filtered and concentrated to give an orange oil. Crystallisation from ethyl acetate/hexane gave dipyrid-2-ylcarbonate as an off-white crystalline solid (3.70 g, 57%).

1. customThe solvent was removed under reduced pressure
2. washwashed with saturated aqueous sodium hydrogen carbonate (2×150 ml) and brine (200 ml)
3. dry with materialdried over anhydrous sodium sulphate
4. filtrationfiltered
5. concentrationconcentrated
6. customto give an orange oil
7. customCrystallisation from ethyl acetate/hexane