反应详情

温度

200 °C

A mixture of 85 (0.7 g, 2.4 mmol) and Pyridine HCl (10 g) was heated to 200° C. After 1 Hr, the reaction was cooled and diluted with water. The aqueous layer was extracted with EtOAc, dried and concentrated to give a solid which was triturated with MeOH, filtered to give a solid (0.5 g, 75%): Mp=184-186° C.; 1H NMR (DMSO-d6) δ 10.04 (s, 1 H), 7.77 (d, 2 H, J=8.3 Hz), 7.67 (t, 1 H, J=0.8 Hz), 7.48-7.46 (m, 1 H), 7.26 (s, 1 H), 6.90 (d, 2H, J=8.2 Hz); MS 277/279 [M−H]−

1. temperatureAfter 1 Hr, the reaction was cooled
2. extractionThe aqueous layer was extracted with EtOAc
3. customdried
4. concentrationconcentrated
5. customto give a solid which
6. customwas triturated with MeOH
7. filtrationfiltered