反应详情

The compound of Example 1 (54.7 mg, 0.124 mmol) and 4-(3-methoxyphenyl)piperidine-1-propanamine (41 mg, 0.165 mmol) were heated together in 2 mL DMF at 100° C. for 16 hours. Water was added into this crude reaction mixture after it was cooled to room temperature and the organic material was extracted with ethyl acetate (3×15 mL). Thin layer chromatography on SiO2 eluted with 10% methanol in methylene chloride showed essentially one single spot. This material was allowed to pass through a short bed of silica gel (Merck Type-H) and the pure product was, recovered as a foam after removal of solvents (43 mg, 54.0%). 1H NMR (DMSO-d6) δ 9.86 (br. s, 1H), 8.93 (br. s, 1H), 7.95 (br. s, 1H), 7.30 (d, 1H, J=7.7 Hz), 7.16 (m, 4H), 6.79 (m, 4H), 4.88 (s, 1H), 3.72 (s, 3H), 3.65 (m, 2H), 3.55 (s, 6H), 3.06 (m, 2H), 2.5 (m, 2H), 2.26 (s, 6H), 1.8 (m, 8H), 13C NMR (DMSO-d6) δ 167.38, 159.31, 145.95, 138.97, 129.36, 118.78, 112.45, 101.08, 54.87, 50.67, 18.28. Anal Calcd. for C36H42N4O7•2.10 H2O: C, 63.53; H, 6.84; N, 8.23. Found: C, 63.48; H, 6.85; N, 8.58.

1. customreaction mixture after it
2. extractionthe organic material was extracted with ethyl acetate (3×15 mL)
3. washThin layer chromatography on SiO2 eluted with 10% methanol in methylene chloride
4. customrecovered as a foam
5. customafter removal of solvents (43 mg, 54.0%)