化学合成。
化学合成
合成路线 1（1. 合成：5281-18-5）
产率：100%
合成条件：With hydrazine hydrate In ethanol at 20℃; for 100 h; Inert atmosphere
实验步骤：在氮气下经10分钟向肼水合物（2.5mL，30mmol）的EtOH（10mL）溶液中滴加苯甲醛（1.04mL，10mmol）。 将得到的溶液在室温下搅拌1.5小时。 此后，加入水并真空蒸发乙醇。 用DCM（x4）萃取水相。 将合并的有机物干燥并浓缩，得到（苯基亚甲基）肼（p2,1.2g，y =定量），为黄色油状物MS（/ T7 / z）：121.1 [MH] +
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合成路线 2（3. 合成：5281-18-5）
产率：55%
合成条件：With hydrazine hydrate In neat (no solvent) for 6 h; Reflux
实验步骤：一般步骤：将DHH的a-h（0.01mol）和过量的水合肼（5mL）的混合物加热回流6小时。 将反应混合物冷却并倒入碎冰中。过滤得到的固体产物a-d，用乙醇结晶，最后干燥。蒸发滤液得到固体残余物，从水中分级结晶得到吡唑和尿素（a）/ 硫脲（b），分别。2.4.1。 3-甲基-1H-吡唑-5-醇（13）。 产率：42-55％（对于a-h）;熔点 熔点221-223℃（Lit. [49]，熔点220-222℃）; 1H-NMR（DMSO-6）δ（ppm）：2.47（s，3H，-CH3），6.83（s，1H，Ar-H），10.07（s，1H，OH），12.10（s，1H，NH））。
参考文献：
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