作为医药中间体或相关化合物的合成原料,用于制备具有特定生物活性的药物分子。
医药
合成路线 1(1. 合成:6492-86-0)
产率:80%
合成条件:With sodium sulfide In acetonitrile at 60℃; for 10 h;
实验步骤:将4-叠氮基-1,8-萘酐(1.8g,7.6mmol)溶于100mL乙腈中,加入硫化钠(6.5g,41mmol)。 加热至60℃保持10小时,冷却,倒入冰水中,抽滤,真空干燥,得到黄色固体1.3g,收率80%。
参考文献:
- [1] Organic and Biomolecular Chemistry, 2015, vol. 13, # 13, p. 3931 - 3935 [2] RSC Advances, 2018, vol. 8, # 21, p. 11419 - 11423 [3] Patent: CN108069967, 2018, A. Location in patent: Paragraph 0011; 0048; 0051; 0052 [4] Journal of Molecular Structure, 2015, vol. 1102, p. 197 - 202 [5] Journal of Materials Chemistry B, 2018, vol. 6, # 18, p. 2860 - 2868
合成路线 2(2. 合成:6492-86-0)
产率:98%
合成条件:With palladium on activated charcoal; hydrogen In acetonitrile at 20℃;
实验步骤:将4-硝基-1,8-萘二甲酸酐(1.26g,5.20mmol)转移至三颈圆底烧瓶中,溶于165mL乙腈中,直至固体完全溶解成棕红色溶液。活性炭上的钯(0.18)将g)加入三颈圆底烧瓶中,将其密封并抽空。在室温和大气压下,在H2下搅拌溶液72小时。然后过滤反应溶液,得到粗产物,其为暗黄色固体,以及催化剂。将粗产物在250mL丙酮中回流并热过滤。重复该过程,合并丙酮的等分试样直至所有粗产物溶解在丙酮中,并通过过滤除去钯催化剂。然后将丙酮溶液通过Celite过滤并通过旋转蒸发除去,得到纯化的产物。 (黄色固体,1.11g,98%)1H NMR(400MHz,d6-DMSO)6.88(d,J = 8Hz,1H),7.69(t,J = 7Hz,1H),7.79(s,2H), 8.19(d,J = 8Hz,1H),8.44(dd,J = 1,7Hz,1H),8.70(dd,J = 1,8Hz,1H)。
参考文献:
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