反应详情

温度

200 °C

A mixture of 82 (0.5 g, 1.9 mmol) and Pyridine HCl (10 g) was heated to 200° C. After 1 hr, the reaction was cooled and then diluted with water. The aqueous layer was extracted with EtOAc, dried over MgSO4 and concentrated to give a solid. The solid was triturated with CH2Cl2 and filtered to give a solid (0.20 g, 47%); Mp=216-218° C.; 1H NMR (DMSO-d6) δ 9.95 (br s, 1 H), 7.74 (d, 2 H, J=8.8 Hz), 7.66 (d, 1 H, J=1.9 Hz), 7.59 (d, 1 H, J=8.8 Hz), 7.27 (dd, 1 H, J=8.8 Hz, 2.4 Hz), 7.17 (s,1 H), 6.88 (d, 2 H, J=8.7 Hz); MS 243/245 [M−H]−

1. temperaturethe reaction was cooled
2. extractionThe aqueous layer was extracted with EtOAc
3. dry with materialdried over MgSO4
4. concentrationconcentrated
5. customto give a solid
6. customThe solid was triturated with CH2Cl2
7. filtrationfiltered