化学合成。
化学合成
合成路线 1(1. 合成:6484-24-8)
产率:73%
合成条件:for 0.25 h; Microwave irradiation
实验步骤:从商业2-甲基喹唑啉-4(3H) - 酮分两步制备分子37。 根据先前微波辅助报道的程序[25],通过使用POCl3,在4位氯化作用最后,导致4-氯-2-甲基喹唑啉,产率为73%。 然后,一般DMAP催化的操作程序在κ3.1.3中描述。 将该产物应用于该中间产物,得到45%收率的分子37,为米色粉末。 熔点118℃,(异丙醇)。 1H NMR(200MHz,CDCl3)δ= 8.33(d,J = 8Hz,1H),7.95-7.83(m,3H),7.65-7.56(m,2H),7.42-7.25(m,2H),2.59 (s,3H),2.47(s,3H)。 13 C NMR(50MHz,CDCl 3)δ= 197.9,166.3,163.7,152.0,150.9,134.3,133.3,132.0,130.1,127.1,127.0,126.0,123.8,123.4,114.3,30.1,26.2。 LC-MS(ESI +)t R 4.60分钟,m / z [M + H] + 279.19。 分子量:278.31g / mol。。 C17H14N2O2的计算值:C,73.37;实测值:73.37。 H,5.07; N,10.07。 实测值:C,73.82; H,5.11; N,9.93。
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