反应详情

Methyl (4-amino-2-fluoro-3-hydroxyphenyl)acetate (996 mg, 5.00 mmol) was dissolved in methanol (50 ml). To the resulting solution was added 1-naphthyl isothiocyanate (926 mg, 5.00 mmol). After the resulting mixture was stirred at room temperature for 2 days, mercuric oxide (yellow) (1.08 g, 5.00 mmol) was added thereto. The mixture was stirred at 70° C. for 3.5 hours. After cooling to room temperature, the reaction mixture was filtered through Celite and washed with methanol. The filtrate was distilled under reduced pressure to remove the solvent. The crude crystals thus obtained were recrystallized from chloroform/n-hexane to give methyl (2-(1-naphthylamino)-7-fluoro-6-benzoxazolyl)acetate (1.41 g, 81%) as a pale gray crystalline powder.

1. stirringThe mixture was stirred at 70° C. for 3.5 hours
2. temperatureAfter cooling to room temperature
3. filtrationthe reaction mixture was filtered through Celite
4. washwashed with methanol
5. distillationThe filtrate was distilled under reduced pressure
6. customto remove the solvent
7. customThe crude crystals thus obtained
8. customwere recrystallized from chloroform/n-hexane