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czjdingyi木虫 (正式写手)
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[交流]
【求助】检索[2.2]Paracyclophane的合成方法
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请大伙帮忙找找[2.2]Paracyclophane的合成方法，Sciencefinder，CA， Beilstein,都行。请将应助结果上传网盘分享。 谢谢了！ [ Last edited by heavence007 on 2009-12-11 at 16:23 ] |
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5楼2009-12-12 10:51:21
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比较可行的路线 (i) H2O, ion-exchange resin Synthetic Communications, 1976 , vol. 6, p. 591 - 596 Full Text With sodium hydroxide Show Experimental Procedure Montedison S.p.A. Patent: US4675462 , 1987 Title/Abstract Full Text EXAMPLE 1 (Comparative Test) Into a 1,000 ml flask equipped with a stirrer, a thermometer and a condenser, there were charged: 100 g of an aqueous solution containing 40percent by weight of NaOH (1 mole), and 62.5 g of an aqueous solution at 63.9percent by weight of p-methylbenzyltrimethylammonium chloride (0.2 moles). Under continuous stirring, the solution was heated by gradually raising the temperature from 22.deg. C. to 120.deg. C. The NaOH concentration was maintained at 35percent by weight. The solution was maintained at the boiling temperature for 5 hours. The resulting (2,2)-paracyclophane was separated from the reaction mass by solubilization in 300 ml of xylene. To this purpose, xylene was added to the reaction mass and the slurry was maintained at total reflux under stirring for 0.5 hour. It was filtered at 95.deg. C., the aqueous phase was separated from the organic solution which was repeatedly washed with water and concentrated to small volume. With sodium hydroxide Show Experimental Procedure Montedison S.p.A. Patent: US4795838 , 1989 Title/Abstract Full Text With iodized misch metal in tetrahydrofuran 1 h; Ambient temperature other metals investigated; Product distribution; Takahashi, Senji; Mori, Nobuo Chemistry Letters, 1989 , p. 13 - 14 Title/Abstract Full Text 22.2% With iodized misch metal in tetrahydrofuran 1 h; Ambient temperature; Takahashi, Senji; Mori, Nobuo Chemistry Letters, 1989 , p. 13 - 14 Title/Abstract Full Text Multi-step reaction with 2 steps 1: 73 percent / NaBH4 / ethanol; tetrahydrofuran / 20 h / 40 °C 2: 1.) isoamyl nitrite, anthranilic acid, 2.) Raney Ni, H2 / 1.) 1,2-dichloroethane, reflux, 4h, 2.) ethanol, reflux, 17-23 h View Scheme Higuchi, Hiroyuki; Misumi, Soichi Tetrahedron Letters, 1982 , vol. 23, # 52 p. 5571 - 5574 Title/Abstract Full Text View citing articles Chow, Hak-Fun; Low, Kam-Hung; Wong, King Y. Synlett, 2005 , # 14 p. 2130 - 2134 Trahanovsky, Walter S.; Lorimor, Steven P. Journal of Organic Chemistry, 2006 , vol. 71, # 5 p. 1784 - 1794 |
4楼2009-12-12 10:43:28
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