请问有人做过将5-甲基-2,2-联吡啶用高锰酸钾氧化成5-羧基-2,2-联吡啶的反应吗?
请问有人做过将5-甲基-2,2-联吡啶用高锰酸钾氧化成5-羧基-2,2-联吡啶的反应吗?按如下文献里的方法做的,但是用盐酸总逼不出固体。。。不知道原因出在何处,恳请各位研友指点迷津,感激不尽!
2,2-Bipyridinyl-5-carboxylic acid (3).11 Potassium permanganate (12.3 g, 78 mmol) was added in 7 portions at 1 h intervals to a solution of 2 (3.4 g, 20 mmol) in water (200 mL). The mixture was heated at 70 C for 3 h and then at 90 C for 4 h more. The brown mixture was then ltered while hot through celite and washed with hot water (2 25 mL). The ltrate was concentrated to approximately 10 mL under reduced pressure, and then 1 M HCl was added slowly until a pH of 4 was obtained. The residue was then ltered and dried to obtain pure 3 (1.2 g, 30%) as a white solid. 1H NMR (400 MHz, DMSO) d 9.19 (s, 1H), 8.76 (d, J ¼ 4.3 Hz, 1H), 8.42–8.54 (m, 3H), 8.01 (t, J ¼ 7.1 Hz, 1H), 7.52–7.55 (m, 1H); 13C NMR (101 MHz, DMSO) d 166.6,
158.8, 154.7, 150.6, 150.0, 138.7, 137.9, 127.0, 125.4, 121.7, 120.7. 返回小木虫查看更多
可能没氧化出来,这个样甲醇酯化后萃取过柱子后,在水解
sorry,我不能查文献,我知道你做的不好做,以前做过类似的,做了两个多月偶尔有几次产率极低,建议你买,或者买溴的插羰后水解,您别说您不懂,不懂可以问老师问同学,我只能点播您一下,您别靠我,要靠你
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