化学合成。
医药
合成路线 1（1. 合成：50270-27-4）
产率：47%
合成条件：Stage #1: for 15 h; Reflux Stage #2: With sodium hydrogencarbonate In water; ethyl acetate
实验步骤：中间体M（1）将嘧啶-2,4,6-三醇（10.0g，78.2mmol），DMF（12mL）在POCl 3（10vol。）中的溶液加热回流15小时。 减压蒸发过量的POCl 3。 将残余物倒入碎冰中。 过滤沉淀的固体并用水洗涤，得到2,4,6-三氯嘧啶-5-甲醛（8.0g，47％），为黄色固体。 该化合物无需进一步纯化即可用于下一步。
参考文献：
- [1] Angewandte Chemie - International Edition, 2006, vol. 45, # 43, p. 7262 - 7265 [2] Patent: WO2012/103297, 2012, A1. Location in patent: Page/Page column 84-85 [3] Patent: WO2017/12576, 2017, A1. Location in patent: Page/Page column 197 [4] Patent: WO2011/14535, 2011, A1. Location in patent: Page/Page column 100 [5] Patent: WO2004/18435, 2004, A1. Location in patent: Page 55-56
合成路线 2（2. 合成：50270-27-4）
产率：88%
合成条件：at 120℃; for 15 h;
实验步骤：将巴比妥酸（5g，78.1mmol）在POCl 3（47mL）和DMF（6mL）中的混合物在120℃加热15小时; 然后真空蒸发，得到浓稠的油状残余物。 在0℃向残余物中加入冰水，得到黄色沉淀。 通过真空过滤收集沉淀物并用水冲洗，得到化合物7A（14.45g，88％）。 1H NMR（CD3Cl）δ11.45（s，1H）。
参考文献：
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