反应详情

温度

0 °C

Compound 38b (0.40 g, 0.57 mmol) was treated with TFA:DCM (1:4 v/v, 15 mL) dropwise with stirring at 0° C. The resulting mixture was stirred for 30 min at rt and concentrated under reduced pressure. The residue obtained was treated with 10 mL of Et2O. The solids formed were collected by filtration and washed with Et2O (2×30 mL) to obtain the title compound 24 as an orange solid. 1H-NMR (300 MHz, DMSO-d6+D2O) δ (ppm): 8.64 (s, 1H), 8.42 (d, J=8.4 Hz, 1H), 8.35 (d, J=9.3 Hz, 1H), 8.21 (d, J=5.4 Hz, 1H), 8.01-7.99 (m, 2H), 7.82 (t, J=15.3 Hz, 1H), 7.70-7.63 (m, 2H), 7.10 (d, J=9.3 Hz, 1H), 6.43 (d, J=5.7 Hz, 1H), 4.16 (s, 2H), 4.02-3.94 (m, 4H), 3.82-3.70 (m, 4H). Mass Spectrum (LCMS, ESI pos.): Calcd. for C28H23N2O3: 506.2 (M+H). Found: 506.1.

1. stirringThe resulting mixture was stirred for 30 min at rt
2. concentrationconcentrated under reduced pressure
3. customThe residue obtained
4. customThe solids formed
5. filtrationwere collected by filtration
6. washwashed with Et2O (2×30 mL)