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以间苯二甲胺和乌洛托品为原料,通过控制反应的pH合成间苯二甲醛。适宜工艺条件为:间苯二甲胺与乌洛托品的摩尔比为1∶4.5、反应温度104℃、反应时间4 h、pH=3~4,在该条件下,收率达76.2%。经IR、1HNMR和ESI-MS表征了产物的结构,确认所得产物即为目标产物,其指标达到国际上对该产品的质量要求,经HPLC测定其色谱纯度为99.7%。
Isophthalamide and methenamine as raw materials, by controlling the pH of the reaction synthesis of isophthalaldehyde. The optimum conditions were as follows: the molar ratio of m - xylenediamine and urotropin was 1: 4.5, the reaction temperature was 104 ℃, the reaction time was 4 h and the pH was 3 ~ 4. Under this condition, the yield was 76.2%. The structure of the product was characterized by IR, 1HNMR and ESI-MS. The obtained product was confirmed to be the target product, and its index reached the international quality requirements for the product. The chromatographic purity was 99.7% as determined by HPLC.