反应详情

The compound of Example 1 (160 mg, 0.364 mmol) and 4-cyclohexyl-1-piperazine-1-propanamine (81.4 mg, 0.362 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 (165 mg, 73.6%): mp 210-212° C.; 1H NMR (DMSO-d6) δ 9.52 (br. s, 1H), 8.91 (br. s, 1H), 7.54 (br. 1H), 7.27 (d, 1H, J=7.3 Hz), 7.16 (m, 2H), 6.80 (d, 1H, J=7.5 Hz), 4.88 (s, 1H), 3.61 (m, 2H), 3.55 (s, 6H), 2.45 (m, 5H), 2.30 (m, 4H), 2.26 (s, 6H), 1.69 (m, 7H), 1.53 (br. d, 1H, J=11.0 Hz), 1.11 (m, 6H); 13C NMR (DMSO-d6) δ 207.50, 207.28, 206.89, 203.73, 199.89, 194.77, 193.47, 192.12, 169.21, 167.38, 163.58, 153.67, 149.15, 145.92, 138.90, 128.87, 121.51, 116.60, 115.86, 101.11, 62.50, 54.94, 53.29, 50.57, 49.90, 48.28, 42.22, 28.32, 27.73, 26.26, 23.50, 18.29, 17.37. Anal Calcd. for C34H45N5O6•0.13 H2O: C, 65.64; H, 7.33; N, 11.26. Found: C, 65.65; H, 7.25; N, 11.09.

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 (165 mg, 73.6%)