反应详情

温度

70 °C

Compound 28b (1.00 g, 3.08 mmol) and 10% Pd on activated carbon (164 mg, 0.154 mmol) were placed in a 40 mL vial equipped with a stir bar and then the vial was evacuated and backflushed with argon. Dry THF (10 mL) was added followed by ammonium formate (388 mg, 6.16 mmol) and then the reaction was stirred at 70° C. for 1 h. The reaction was cooled to rt and diluted with DCM (200 mL). The solids were removed by filtration and then washed with DCM (2×50 mL). The combined filtrates were concentrated under reduced pressure to afford compound 28c. 1H-NMR (400 MHz, CDCl3) δ (ppm): 7.96 (d, J=5.1 Hz, 1H), 7.80 (s, 1H), 6.02 (d, J=5.1 Hz, 1H), 4.21 (q, J=6.8 Hz, 2H), 3.85-4.01 (m, 8H), 3.83 (s, 2H), 1.29 (t, J=6.8 Hz, 3H). Mass Spectrum (LCMS, ESI pos.) Calcd. For C14H18N4O3: 291.2 (M+H). Found: 291.1.

1. customvial equipped with a stir bar
2. customthe vial was evacuated
3. additionDry THF (10 mL) was added
4. temperatureThe reaction was cooled to rt
5. customThe solids were removed by filtration
6. washwashed with DCM (2×50 mL)
7. concentrationThe combined filtrates were concentrated under reduced pressure