化学合成。
化学合成
合成路线 1(1. 合成:25477-96-7)
产率:20%
合成条件:With potassium carbonate In water; N,N-dimethyl-formamide
实验步骤:实施例26 9-羧甲基腺嘌呤乙酯的合成将腺嘌呤(10g,74mmol)和碳酸钾(10.29g,74mmol)悬浮于DMF中,加入溴乙酸乙酯(8.24mL,74mmol)。将该悬浮液在室温下在氮气下搅拌2.5小时,然后过滤。将固体残余物用DMF(10mL)洗涤三次。将合并的滤液真空蒸发至干。将水(200mL)加入到黄橙色固体物质中,并用4N HCl将pH调节至6。在0℃下搅拌10分钟后,滤出固体,用水洗涤,并从96%乙醇(150mL)中重结晶。过滤分离标题化合物,用乙醚彻底洗涤。产量:3.4克(20%)。熔点215.5-220℃。。得到的C9H11N5O2(计算值):C:48.86(48.65); H:5.01(4.91); N:31.66(31.42)。 1H-NMR(250MHz; DMSO-d6):7.25(bs,2H,NH),5.06(s,2H,NCH2),4.17(q,2H,J = 7.11Hz,OCH2)和1.21(t,3H, J = 7.13Hz,NCH2)。 13 C-NMR。 152.70,141.30,61.41,43.97和14.07。 FAB-MS。 222(MH +)。 IR:频率,单位为cm-1(强度)。 3855(54.3),3274(10.4),3246(14.0),3117(5.3),2989(22.3),2940(33.9),2876(43.4),2753(49.0),2346(56.1),2106(57.1), 1899(55.7),1762(14.2),1742(14.2),1742(1.0),1671(1.8),1644(10.9),1606(0.6),1582(7.1),1522(43.8),1477(7.2), 1445(35.8)和1422(8.6)。
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