反应详情

温度

200 °C

A mixture of 81 (0.3 g, 1 mmol) and Pyridine HCl (5 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 (0.11 g, 39%); Mp=228–229° C.; 1H NMR (DMSO-d6) δ 9.95 (br s, 1 H), 7.79 (d, 1 H, J=2.0 Hz), 7.74 (d, 2 H, J=8.8 Hz), 7.55 (d, 1 H, J=8.8 Hz), 7.39 (dd, 1 H, J=8.8 Hz, 2.4 Hz), 7.16 (s, 1 H), 6.88 (d, 2 H, J=8.8 Hz); MS 287/289[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