反应详情

温度

200 °C

A mixture of 74 (1.5 g, 5.2 mmol) and Pyridine HCl (10 g) was heated to 200° C. After 1.5 hr, the reaction was cooled and diluted with water. The aqueous layer was extracted with EtOAc and the organic layer was dried, concentrated to give a solid which was triturated with CH2Cl2 to give a solid (0.6 g, 51%): Mp=275–278° C.; 1H NMR (DMSO-d6) δ 9.81 (br s, 1 H), 9.12 (br s, 1 H), 7.66 (d, 2 H, J=2.5 Hz), 7.32 (d, 1 H, J=8.5 Hz), 7.00 (s, 1 H), 6.90–6.83 (m, 3 H), 6.65 (dd, 1 H, J=8.6 Hz, 2.6 Hz); MS 225 (M−H)−.

1. temperaturethe reaction was cooled
2. extractionThe aqueous layer was extracted with EtOAc
3. customthe organic layer was dried
4. concentrationconcentrated
5. customto give a solid which
6. customwas triturated with CH2Cl2