2,4-二氨基-1,3,5-三嗪可用作医药合成中间体,如制备如下化合物:
具体步骤...
1)5-氯-3-(环己-1-烯-1-基)-7-甲氧基-6-(4-甲氧基苯基)-2-苯基吡唑并[1,5-a]嘧啶(222g,0.5mmol),2,4-二氨基-1,3,5-三嗪(83mg,0.75mmol,1.5当量),Pd(OAc)2(23mg,0.1mmol,0.2当量),Xantphos(115mg,0.2mmol,0.4)eq.)和Cs2CO3(195mg,0.6mmol,12当量)在1.4mL二恶烷(4mL)中,在100℃下通过微波辐射在N2气氛下加热1小时.LC-MS:m/z521.0(M+H)+.
2)N2-(3-(环己-1-烯-1-基)-7-甲氧基-6-(4-甲氧基苯基)-2-苯基吡唑并[1,5-a]嘧啶的溶液-5-氯-1,5-三嗪-2,4-二胺(80mg,0.15mmol)的HCl1,4-二恶烷(5mL)溶液.在室温下搅拌溶液.6小时在真空中除去溶剂和挥发物.将残余物溶于DCM(5mL)中并用饱和NaHCO3处理.分离有机相并用盐水洗涤,经无水Na2SO4干燥并真空浓缩,得到标题化合物.
1HNMR(DMSO-d6): δ8.28(br.s,1H), 7.74(d,J=7.2Hz,2H), 7.38-7.52(m,4H), 7.31(d,J=8.2)Hz,2H), 7.03(d,J=8.2Hz,2H), 5.96(br.s.,1H), 3.80(s,3H), 2.26(br.s.,2H), 2.04(br.s.,2H), 1.68(br.s.,4H).
LC-MS:m/z507.0(M+H)+.
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