反应详情

Potassium carbonate (4.6 g, 33.3 mmol) was added to a solution of N-(2-fluoro-4-chloro-5-methoxycarbonyloxyphenyl)-3,4,5,6-tetrahydrophthalimide (11.8 g, 33.4 mmol) obtained as described above in methanol (100 ml), followed by stirring for 5 hours under refluxing. After completion of the reaction, the mixture was poured into 1N hydrochloric acid (200 ml), and the mixture was extracted with ethyl acetate (100 ml×3 times). The organic layer was washed with water, dried, and the solvent was distilled off under reduced pressure to obtain a crude product (9.4 g). The product was recrystallized from ether/hexane to obtain N-(2-fluoro-4-chloro-5-hydroxypheyl) 3,4,5,6-tetrahydrophthalimide as a white solid (6.7 g 22.7 mmol, 67.8% yield).

1. customobtained
2. temperatureunder refluxing
3. customAfter completion of the reaction
4. extractionthe mixture was extracted with ethyl acetate (100 ml×3 times)
5. washThe organic layer was washed with water
6. customdried
7. distillationthe solvent was distilled off under reduced pressure
8. customto obtain a crude product (9.4 g)
9. customThe product was recrystallized from ether/hexane