将12.4 g化合物10和6.9 g的化合物11、17.4 g的K2CO3加入到86 mL CH3CN中, 65 ℃加热回流, 反应6 h后, TLC监测原料反应完毕, 停止反应, 待体系温度降至室温, 过滤除去体系中的固体, 收集滤液, 滤饼用DCM洗涤, 合并有机相并减压浓缩除去溶剂, 得18.7 g黄色固体.对所得产物粗品用乙醇进行洗涤后进行重结晶:向体系中加入10 mL乙酸乙酯稀释, 75 ℃加热回流, 后缓慢加入乙酸乙酯直至体系刚刚澄清透明, 自然降至室温, 有白色固体析出, 减压抽滤, 收集滤饼, 并将所得固体真空干燥, 得白色固体粉末8.6 g, 收率为56%.即TJAB1099. m.p. 135.4~136.9 ℃; 1H NMR (400 MHz, Chloroform-d) δ: 8.04 (s, 1H), 7.96 (d, J=5.9 Hz, 1H), 7.47~7.55 (m, 2H), 6.9~6.98 (m, 1H), 6.84~6.91 (m, 2H), 6.74 (dd, J=6.0, 2.0 Hz, 1H), 4.38 (s, 2H), 4.18~4.26 (m, 2H), 4.00~4.10 (m, 2H), 3.69~3.81 (m, 2H), 3.45~3.54 (m, 2H), 3.29~3.43 (m, 2H), 1.74~1.93 (m, 2H), 1.63~1.74 (m, 2H), 1.41~1.51 (m, 1H), 1.34 (t, J=7.1 Hz, 3H), 1.05 (d, J=6.4 Hz, 3H); 13C NMR (101 MHz, Chloroform-d) δ: 160.22, 159.36, 156.93, 148.65, 148.47, 147.95, 128.39, 124.98, 114.61, 102.79, 94.74, 69.54, 65.89, 41.77, 41.54, 41.34, 35.92, 34.16, 27.50, 19.46, 14.63; IR (KBr) ν: 3418.06, 3294.25, 3157.71, 2931.26, 2879.04, 1699.9, 1689.97, 1641.06, 1606.71, 1547.88, 1506.67, 1482.88, 1376.71, 1250.65, 1055.84, 961.97, 825.75 cm-1; HR-MS calcd for C23H32N5O3 [M+H]+ 426.5330, found 426.5303.
化学慧定制合成事业部