反应详情

温度

100 °C

Iron powder (6.08 g, 109 mmol) was added to a solution of 4-chloro-2-(2-chloro-6-nitrophenyl)thiazolo[5,4-c]pyridine (3.55 g, 10.9 mmol) in AcOH (100 mL). The reaction mixture was heated at 100° C. for 30 minutes and then allowed to cool to room temperature. The volatiles were removed under reduced pressure and the resultant residue was dissolved in DCM/MeOH and filtered through Celite® washing further with MeOH. The combined washings were concentrated under reduced pressure and the resultant residue was triturated with 10% MeOH in DCM to afford the title compound as an orange/red solid (2.55 g, 79% yield). 1H NMR (400 MHz, CDCl3): δ 8.44 (d, J=5.6 Hz, 1H), 7.83 (d, J=5.7 Hz, 1H), 7.16 (t, J=7.9 Hz, 1H), 6.89 (dd, J=1.2, 7.8 Hz, 1H), 6.73 (dd, J=1.2, 8.3 Hz, 1H), 6.14 (br s, 2H).

1. temperatureto cool to room temperature
2. customThe volatiles were removed under reduced pressure
3. dissolutionthe resultant residue was dissolved in DCM/MeOH
4. filtrationfiltered through Celite®
5. washwashing further with MeOH
6. concentrationThe combined washings were concentrated under reduced pressure
7. customthe resultant residue was triturated with 10% MeOH in DCM