將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 ℃加熱回流, 反應(yīng)6 h后, TLC監(jiān)測(cè)原料反應(yīng)完畢, 停止反應(yīng), 待體系溫度降至室溫, 過濾除去體系中的固體, 收集濾液, 濾餅用DCM洗滌, 合并有機(jī)相并減壓濃縮除去溶劑, 得18.7 g黃色固體.對(duì)所得產(chǎn)物粗品用乙醇進(jìn)行洗滌后進(jìn)行重結(jié)晶:向體系中加入10 mL乙酸乙酯稀釋, 75 ℃加熱回流, 后緩慢加入乙酸乙酯直至體系剛剛澄清透明, 自然降至室溫, 有白色固體析出, 減壓抽濾, 收集濾餅, 并將所得固體真空干燥, 得白色固體粉末8.6 g, 收率為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.
化學(xué)慧定制合成事業(yè)部
