6813-38-3 2,2'-联吡啶-4,4'-二甲酸

危险性质：非危险化学品

化学合成；材料科学。

2,2'-联吡啶-4,4'-二甲酸为羧酸类衍生物，可用作医药中间体。

合成路线 1（1. 合成：6813-38-3）

产率：98% 合成条件：at 65℃; for 6 h; 实验步骤：将1.0g的4,4-二甲基-2,2-联吡啶（5.4mmol）加入到反应烧瓶中，缓慢滴加18mL浓硫酸并搅拌，该过程大量加热直至溶液冷却至室温 然后加入重铬酸钾3.3g（11.3mmol），然后溶液变为深绿色，然后在65℃反应6小时。 反应完成并冷却至室温，反应物加入1000mL水中，此时产生大量白色絮状沉淀，抽滤，然后用水和甲醇洗涤，滤液呈白色沉淀澄清。 然后在真空烘箱中于60±18h干燥，产率98％ 参考文献：

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合成路线 2（2. 合成：6813-38-3）

产率：85% 合成条件：With hydrogenchloride; sodium hydroxide In methanol; water 实验步骤：实施例5将5.00g 2-氯异烟酸和2.80g氢氧化钠溶于20ml水和16ml甲醇的混合物中。 在加入1.02g钯（活性炭重量百分比为10％）作为催化剂后，将混合物在80-85℃，0.1MPa下搅拌6小时。 然后滤除催化剂。 用盐酸酸化至pH1后，产物2,2'-联吡啶-4,4'-二羧酸沉淀出白色固体。 得到3.3g（收率85％）。 参考文献：

• [1] Patent: US6500956, 2002, B1

合成路线 3（3. 合成：6813-38-3）

产率：45% 合成条件：With nitric acid In water at 180℃; for 36.17 h; Heating 实验步骤：将4,4'，6,6'-四羧基-2,2'-联吡啶（0.083g; 0.25mmol）置于45mlTeflon衬里的消化炸弹在H 2 O（8ml）中并浓缩。 HNO3（1ml）。 将其搅拌10分钟，密封，加热至180℃，保持36小时，并以5℃/小时的速率冷却。 参考文献：

• [1] Inorganica Chimica Acta, 2013, vol. 403, p. 102 - 109