反应详情

The compound of Example 2 (98.3 mg, 0.215 mmol) and 4-(3-methoxyphenyl)piperidine-1-propanamine (64 mg, 0.258 mmol) were stirred in 2 mL DMF at room temperature for 64 hours. The crude reaction mixture was evaporated to dryness under high vacuum (0.1 mmHg) at 50-55° C. The resulting gum was triturated with methylene chloride followed by the addition of hexanes. The titled compound precipitated out as fine creamy white crystalline solid (120 mg, 84.6%): mp 205-207° C.; 1H NMR (DMSO-d6) δ 9.38 (br. s, 1H), 8.96 (br. s, 1H), 8.04 (br. t, 1H, J=3 Hz), 7.80 (d, 1H, J=7.2 Hz), 7.10 (m, 2H), 6.77 (m, 4H), 4.85 (s, 1H), 3.71 (s, 3H), 3.65 (q, 2H, J=6.0 Hz), 3.53 (s, 6H), 2.95 (d, 2H, J=10.5 Hz), 2.40 (m, 3H), 2.25 (s, 6H), 1.97 (m, 2H), 1.67.(m, 6H), 13C NMR (DMSO-d6) δ 184.94, 179.65, 169.52, 167.32, 163.03, 159.26, 147.95, 146.23, 145.07, 129.25, 126.76, 126.62, 119.68, 118.81, 114.66, 114.40, 112.41, 111.35, 100.93, 55.14, 54.83, 53.73, 50.60, 32.93, 27.84, 18.31. Anal Calcd. for C36H41 FN4O7•0.14 H2O: C, 65.19; H, 6.27; N, 8.45. Found: C, 65.20; H, 6.28; N, 8.37.

1. customThe crude reaction mixture
2. customwas evaporated to dryness under high vacuum (0.1 mmHg) at 50-55° C
3. customThe resulting gum was triturated with methylene chloride
4. additionfollowed by the addition of hexanes
5. customThe titled compound precipitated out as fine creamy white crystalline solid (120 mg, 84.6%)