反应详情

Example 33 (0.90 g, 2.8 mmol) and Pyr-HCl (5 g) were heated together at 200° C. for 2 h. The reaction was cooled and diluted with water and the resultant solid filtered off. The solid thus obtained was triturated with MeOH, filtered, and triturated with EtOAc and then CH2Cl2. The resulting pink solid was dissolved in CH3OH/EtOAc (200 mL) and silica gel added. The solution was filtered and concentrated and the resulting solid triturated with CH3OH and then CH2Cl2. The product 36 was isolated as an off-white solid (0.35 g): Mp>300° C.; 1H NMR (DMSO-d6) δ 12.71 (s, 1H), 10.88 (s, 1H), 10.71 (s, 1H), 7.85 (d, 1H, J=8.7 Hz), 7.12 (d, 1H, J=1.8 Hz), 7.0 (dd, 1H, J=8.7 Hz, 1.9 Hz), 6.56 (d, 1H, J=2.1 Hz), 6.27 (d, 1H, J=2.0 Hz); MS 283 (M−H)−.

1. customwere heated together at 200° C. for 2 h
2. temperatureThe reaction was cooled
3. filtrationthe resultant solid filtered off
4. customThe solid thus obtained
5. customwas triturated with MeOH
6. filtrationfiltered
7. customtriturated with EtOAc
8. dissolutionThe resulting pink solid was dissolved in CH3OH/EtOAc (200 mL)
9. additionsilica gel added
10. filtrationThe solution was filtered
11. concentrationconcentrated
12. customthe resulting solid triturated with CH3OH