反应详情

温度

70 °C

n-Bromohexane (0.077 ml, 0.55 mmol, 1.05 equiv.) was added to a suspension of 2-[3-(aminocarbonyl)-2,4-difluorophenoxy]acetic acid (120 mg, 0.52 mmol, 1 equiv.) and K2CO3 (215 mg, 1.56 mmol, 3 equiv.) in DMF (3 ml) and the mixture was stirred at 70° C. for 1.5 h. After cooling at r.t., the mixture was poured into water (25 ml) and the precipitant solid was filtered and washed with water (2×20 ml). After drying, the crude solid was triturated by stirring in hexane (10 ml), filtered and washed with hexane (3×10 ml), to give the desired compound as a white solid (99 mg, 60%), mp 108° C. HPLC-MS: m/z 316 [M+H]+, Rt=4.09 min.

1. temperatureAfter cooling at r.t.
2. filtrationthe precipitant solid was filtered
3. washwashed with water (2×20 ml)
4. customAfter drying
5. customthe crude solid was triturated
6. stirringby stirring in hexane (10 ml)
7. filtrationfiltered
8. washwashed with hexane (3×10 ml)