反应详情

A solution of 5-[1-(4-hydroxyphenyl)but-2-ynyl]-2,2-dimethyl-1,3-dioxane-4,6-dione (20 g, 69.44 mmol) in pyridine-water (5:1, 390 mL) is heated at reflux for 16 hours and after cooling is acidified to pH ˜2 with 5 N HCl and extracted with EtOAc (2×300 mL). The combined extracts are washed with saturated brine, dried over MgSO4, filtered, and concentrated to give an off-white solid (13.5 g, 96%). ESI/MS m/z 203 (M−H)−.

1. temperatureat reflux for 16 hours
2. temperatureafter cooling
3. extractionextracted with EtOAc (2×300 mL)
4. washThe combined extracts are washed with saturated brine
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated