反应详情

To a stirring solution of 2-(5-(2-(benzyloxy)-1,1,1-trifluoropropan-2-yl)-1,3,4-oxadiazol-2-yl)-6-methoxy-5-(trifluoromethyl)pyridin-3-amine trifluoroacetate (Step 3) (450 mg, 0.973 mmol) in EtOH (25 ml) was added palladium hydroxide on carbon (45.1 mg, 0.321 mmol) followed by ammonium formate (614 mg, 9.73 mmol). The mixture was heated at reflux for 1 h and then filtered through Celite® washing through with EtOH followed by water. The ethanol was removed in vacuo and the resultant aqueous phase was extracted with EtOAc. The combined organic extracts were washed with water, brine, dried (MgSO4) and concentrated in vacuo to afford the title product; 1H NMR (400 MHz, DMSO-d6) δ 7.85 (1H, s), 7.74 (1H, s), 6.74 (2H, s), 3.94 (3H, s), 1.86 (3H, s). LC-MS Rt=1.17 min [M+H]+ 373.1 Method: 2minLC_v003.

1. temperatureThe mixture was heated
2. temperatureat reflux for 1 h
3. filtrationfiltered through Celite®
4. washwashing through with EtOH
5. customThe ethanol was removed in vacuo
6. extractionthe resultant aqueous phase was extracted with EtOAc
7. washThe combined organic extracts were washed with water, brine
8. dry with materialdried (MgSO4)
9. concentrationconcentrated in vacuo