反应详情

Into a round bottom flask were added tert-Butyl 4-(4-{7-[1-(2,6-dichloro-3,5-difluorophenyl)ethoxy]-6-nitrofuro[3,2-c]pyridin-3-yl}-1H-pyrazol-1-yl)piperidine-1-carboxylate (220 mg, 0.34 mmol), iron (192 mg, 3.44 mmol), 2 drops of 0.1 M HCl and EtOH (7 mL), and the reaction mixture was refluxed for 30 min. 0.1 M HCl was added dropwise and reaction refluxed until consumption of SM was observed. Reaction was stopped and filtered through silica gel washing with 5% MeOH in DCM. Reaction mixture was concentrated in vacuo to obtain the title compound. MS (ES+): m/z 608.06/610.07 (100/70) [MH+]. HPLC: tR=3.74 min (ZQ3, polar—5 min).

1. temperaturethe reaction mixture was refluxed for 30 min
2. customreaction
3. temperaturerefluxed until consumption of SM
4. customReaction
5. filtrationfiltered through silica gel washing with 5% MeOH in DCM
6. customReaction mixture
7. concentrationwas concentrated in vacuo