反应详情

A solution of compound 42b (0.10 g, 0.18 mmol) and 2,3,4,6,7,8,9,10-octahydropyrimido[1,2-a]azepine (0.10 g, 0.66 mmol) in o-xylene (2 mL) was stirred at 130° C. in an oil bath for 2 h. The reaction mixture was allowed to cool to rt, and the solution was adjusted to pH 7 with 0.5 N HCl. The solids formed were collected by filtration and washed with CH2Cl2/MeOH (1:10) (3×10 mL) to obtain the title compound 26 as a brown solid. 1H-NMR (300 MHz, DMSO-d6) δ (ppm): 13.25 (s, 1H), 9.48 (s, 1H), 8.79-8.75 (m, 1H), 8.47 (d, J=8.4 Hz, 1H), 8.33 (d, J=5.7 Hz, 1H), 8.24 (d, J=8.7 Hz, 1H), 8.06-8.01 (m, 2H), 7.87-7.66 (m, 3H), 7.56 (d, J=6.0 Hz, 1H), 4.10-3.98 (m, 4H), 3.91-3.78 (m, 4H). Mass Spectrum (LCMS, ESI pos.): Calcd. for C28H20N8O3: 517.2 (M+H). Found: 517.1.

1. customThe solids formed
2. filtrationwere collected by filtration
3. washwashed with CH2Cl2/MeOH (1:10) (3×10 mL)