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2-Hydroxy-l，3-bis(1-pyridinium)propanebisperchlorate 。A solution of pyridinium perchlorate (1.8 g, ), pyridine （0.8 g), and epichlorohydrin (0.8 ml, ) in ethanol(80 ml) was refluxed for 5 h, cooled, and HClO4 (57%, 1 ml) added. After standing overnight at -15°c the precipitate was separated,washed with cold alcohol, and dried at 100°c to give 3 g (72%). The mother liquor contained a further 0.5 g of colored material. The colorless crystals had mp 158-160°c (from ethanol). PMR Spectrum: 4~67-5.67 (SH, m, Alk); 7.2-9.2 ppm (10H, m, At). The same material could be obtained in quantitative yield by refluxing the salt and pyridine for 2-3 h in ethanol. |
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2楼2010-03-04 21:20:43
xiaoqihu
铁杆木虫 (著名写手)
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phyweiw(金币+2):协助版主工作奖励 2010-03-04 21:54
wyq4504(金币+5): 2010-03-05 08:57
phyweiw(金币+2):协助版主工作奖励 2010-03-04 21:54
wyq4504(金币+5): 2010-03-05 08:57
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2-Hydroxy-l，3-bis(1- pyridinium)propanebisperchlorate的合成 pyridinium perchlorate (1.8 g, ), 吡啶 （0.8 g), 和epichlorohydrin (0.8 ml, )的乙醇溶液(80 ml)回流5小时，冷却后加入HClO4 (57%, 1 ml)，-15°c 下放置过夜，分理出析出物，用冷的乙醇洗涤，然后将其放置于100°c下干燥，得到3 g (72%)产物，母液里进一步得到0.5 g有颜色的产物。无色产物的mp 158-160°c，PMR Spectrum: 4~67-5.67 (SH, m, Alk); 7.2-9.2 ppm (10H, m, At). 回流盐和吡啶的乙醇溶液2-3小时可以定量的得到同样的产物 PMR Spectrum？？？？ 孙便请教一下PMR Spectrum？？？？是什么？ [ Last edited by xiaoqihu on 2010-3-4 at 22:47 ] |
3楼2010-03-04 21:44:16
wyq4504(金币+5): 2010-03-05 08:57
| 2-Hydroxy-l，3-bis(1-pyridinium)propanebisperchlorate 。A solution of pyridinium perchlorate (1.8 g, ), pyridine （0.8 g), and epichlorohydrin (0.8 ml, ) in ethanol(80 ml) was refluxed for 5 h. After cooled, 1 ml HClO4 (57%,) was added and the mixture was kept aside overnight at -15°c . The precipitate was separated and washed with cold alcohol and dried at 100°c to yield 3 g (72%). The mother liquor contained a further 0.5 g of colored material. The colorless crystals had mp 158-160°c (from ethanol). PMR Spectrum: 4~67-5.67 (SH, m, Alk); 7.2-9.2 ppm (10H, m, At). The same material could be obtained in quantitative yield by refluxing the salt and pyridine for 2-3 h in ethanol. |
4楼2010-03-04 21:46:21
5楼2010-03-04 21:53:49
xiaoqihu
铁杆木虫 (著名写手)
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6楼2010-03-04 22:41:37
7楼2010-03-05 08:57:06