131543-46-9
492-98-8
以化合物(CAS:131543-46-9)為起始原料,合成1H,1'H-2,2'-聯(lián)咪唑的一般步驟如下:首先,在40℃條件下,向1,092g(14.2mol,4.0當量)乙酸銨中加入120ml蒸餾水,隨后緩慢加入500g 20wt%乙二醛水溶液(3.45mol)。在劇烈攪拌下,將所得漿液滴加3小時。滴加完畢后,立即用蒸餾水中和反應混合物,調節(jié)pH至5-7。過濾生成的棕色固體,并依次用500ml丙酮和500ml蒸餾水交替洗滌數(shù)次,最終得到82.0g(產率53.2%)純度未達97%的2,2'-二-1H-咪唑。
參考文獻:
[1] Patent: US2003/199700, 2003, A1. Location in patent: Page/Page column 2
[2] Patent: US2003/199700, 2003, A1. Location in patent: Page/Page column 2
[3] Archiv der Pharmazie, 1986, vol. 319, # 2, p. 183 - 185
[4] Patent: US2003/199700, 2003, A1. Location in patent: Page/Page column 2
[5] Patent: US2003/199700, 2003, A1. Location in patent: Page/Page column 2