反应详情

A mixture of anisole (288 μl, 2.66 mmol), trifluoroacetic acid (10 ml), and ethyl (5-chloro-2-fluoro-4-(1-(4-methoxybenzyl)-3-indazolylcarbonylamino)phenyl)acetate (880 mg, 1.77 mmol) was heated under reflux for 15 hours. After cooling, the reaction mixture was distilled under reduced pressure to remove the solvent. Water (50 ml) was added to the residue. The crystals thus precipitated were collected by filtration under reduced pressure and washed with water. The crude crystals thus obtained were recrystallized from chloroform-methanol, whereby ethyl (5-chloro-2-fluoro-4-(3-indazolylcarbonylamino)phenyl)acetate (531 mg, 80%) was obtained as a colorless crystalline powder.

1. temperaturewas heated
2. temperatureunder reflux for 15 hours
3. temperatureAfter cooling
4. distillationthe reaction mixture was distilled under reduced pressure
5. customto remove the solvent
6. additionWater (50 ml) was added to the residue
7. customThe crystals thus precipitated
8. filtrationwere collected by filtration under reduced pressure
9. washwashed with water
10. customThe crude crystals thus obtained
11. customwere recrystallized from chloroform-methanol