反应详情

温度

60 °C

TMSI (100 μL, 0.734 mmol) was added to a solution of 2′-methoxy-N-(4-(trifluoromethoxy)phenyl)-[3,3′-bipyridine]-5-carboxamide (Example 62, 79 mg, 0.203 mmol) in CHCl3 (4 mL) and the RM was stirred at 60° C. overnight. The RM was cooled to RT, poured into MeOH and the solvent was evaporated off under reduced pressure. The residue was treated with aq. 5% NH3 and extracted with EtOAc. The combined extracts were washed with brine, dried over Na2SO4 and the solvent was evaporated off under reduced pressure to give the product which was recrystallized from hot EtOAc to afford the title compound as beige crystals. UPLC-MS (Condition 2) tR0.87 min, m/z=376.1 [M+H]+; 1H-NMR (400 MHz, DMSO-d6) δ ppm 6.38 (t, J=6.65 Hz, 1H) 7.40 (d, J=8.99 Hz, 2H) 7.51 (d, J=6.26 Hz, 1H) 7.86-7.96 (m, 3H) 8.61-8.66 (m, 1H) 9.00-9.04 (m, 1H) 9.09-9.13 (m, 1H) 10.63 (s, 1H) 12.03 (br. s, 1H).

1. temperatureThe RM was cooled to RT
2. customthe solvent was evaporated off under reduced pressure
3. additionThe residue was treated with aq. 5% NH3
4. extractionextracted with EtOAc
5. washThe combined extracts were washed with brine
6. dry with materialdried over Na2SO4
7. customthe solvent was evaporated off under reduced pressure
8. customto give the product which
9. customwas recrystallized from hot EtOAc