化学合成。
化学合成
合成路线 1(1. 合成:7306-68-5)
产率:99.3%
合成条件:With toluene-4-sulfonic acid In ethyl acetate at 90℃; for 1 h;
实验步骤:将6-氯-9H-嘌呤(25.36g,164mmol)和4-甲基苯磺酸(0.565g,3.28mmol)的EtOAc(250mL)悬浮液用3,4-二氢-2H-吡喃(44.9mL)处理 ,492mmol)。 将混合物在90℃下加热,并将固体在1小时内缓慢溶解。 从油浴中取出烧瓶,过滤混浊的黄色溶液并真空浓缩。 将浅黄色残余物溶于DCM中,并通过快速色谱法(50%EtOAc /己烷)(1L二氧化硅/ 4L溶剂)纯化,得到6-氯-9-(四氢-2H-吡喃-2-基)-9H-嘌呤。 (38.90g,99.3%收率),为无色油状物,其缓慢结晶。 MS(ESI,阳离子)m / z:239.1 [M + H] +
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