反应详情

A reactor was charged with DMF (68 Kg), and stirring was initiated. The reactor was then charged with phenol (51 Kg), acetylacetone (8 Kg), 5-bromophthalide (85 Kg), copper bromide (9 Kg), and potassium carbonate (77 Kg). The mixture was heated above 85° C. and maintained until reaction completion and then cooled. Water was added. Solid was filtered and washed with water. Solid was dissolved in dichloromethane, and washed with aqueous HCl and then with water. Solvent was removed under pressure and methanol was added. The mixture was stirred and filtered. Solid was washed with methanol and dried in an oven giving 5-phenoxyphthalide (Yield: 72%, HPLC: 99.6%).

1. temperatureThe mixture was heated above 85° C.
2. temperaturemaintained until reaction completion
3. temperaturecooled
4. filtrationSolid was filtered
5. washwashed with water
6. dissolutionSolid was dissolved in dichloromethane
7. washwashed with aqueous HCl
8. customSolvent was removed under pressure and methanol
9. additionwas added
10. stirringThe mixture was stirred
11. filtrationfiltered
12. washSolid was washed with methanol
13. customdried in an oven