医药中间体;化学合成原料;材料科学用试剂
医药;化学合成;材料科学
路线1:以[2,2'-联吡啶]-4,4'-二甲酸二乙酯为原料
- 步骤:将硼氢化钠(1.87g,49mmol)加入到溶解在无水乙醇(34mL)中的[2,2'-联吡啶]-4,4'-二羧酸二乙酯(567mg,1.89mmol)的悬浮液中;回流3小时;冷却至室温后,加入饱和氯化铵溶液(24mL/g NH₄Cl)分解过量硼氢化钠;真空蒸发乙醇,超声浴将所得固体溶于最少量水中;乙酸乙酯(5×34mL)萃取,硫酸钠干燥,真空浓缩得白色粉末。
- 收率:91%
- 参考文献:[1] Chemical Communications, 2009, #48, p.7545-7547;[2] Electrochimica Acta, 2016, vol.207, p.313-320;[3] Journal of Physical Chemistry B, 1999, vol.103, #38, p.8067-8079;[4] Patent: CN105793241, 2016, A. Location in patent: Paragraph 0129; 0159;[5] Tetrahedron, 2014, vol.70, #36, p.6271-6275;[6] Dalton Transactions, 2015, vol.44, #12, p.5577-5586;[7] Polyhedron, 2013, vol.57, p.52-56;[8] Inorganic Chemistry, 2017, vol.56, #3, p.1366-1374;[9] Tetrahedron Letters, 2010, vol.51, #47, p.6161-6165;[10] Journal of Chemical Sciences, 2011, vol.123, #1, p.37-46;[11] Inorganic Chemistry, 2015, vol.54, #9, p.4512-4519;[12] Journal of the American Chemical Society, 2012, vol.134, #2, p.968-978;[13] Spectrochimica Acta - Part A: Molecular and Biomolecular Spectroscopy, 2016, vol.165, p.150-154;[14] Green Chemistry, 2014, vol.16, #9, p.4179-4189;[15] Chemistry - A European Journal, 2017, vol.23, #72, p.18239-18251