4354-73-8 2-环己基亚己基丙二腈

运输信息：常温运输。危险描述：非危险化学品。

化学合成。

化学合成

合成路线 1（1. 合成：4354-73-8）

产率：100% 合成条件：at 25℃; for 2 h; 实验步骤：相应的反应（a）至（p）是通过在搅拌下和在5ml溶剂（二甲基甲酰胺（己烷）DMF或乙腈（MeCN））中，1毫摩尔羰基化合物和1毫摩尔活化甲醇的反应实现的。 在实施例1中制备0.0035g'HDT-F'催化剂。在每种情况下，通过在板上进行色谱法跟踪反应进程。 在反应结束时，过滤催化剂，滤液用水洗涤，产物用硫酸钠萃取并在低压下浓缩。 基于在最终培养基中观察到的NMR光谱，基于反应过程中消耗的R1R2CO酮化合物计算所示产率。 参考文献：[1] Patent: US2005/250963, 2005, A1. Location in patent: Page/Page column 5 [2] Green Chemistry, 2010, vol. 12, # 3, p. 514 - 517 [3] Synlett, 2000, # 7, p. 1016 - 1018 [4] Collection of Czechoslovak Chemical Communications, 2005, vol. 70, # 10, p. 1727 - 1736 [5] European Journal of Organic Chemistry, 2008, # 28, p. 4763 - 4768 [6] RSC Advances, 2013, vol. 3, # 45, p. 23075 - 23079 [7] Russian Chemical Bulletin, 2013, vol. 62, # 3, p. 683 - 686 [8] Izv. Akad. Nauk, Ser. Khim., 2013, # 3, p. 682 - 685,4 [9] Journal of the Chinese Chemical Society, 2013, vol. 60, # 3, p. 288 - 292 [10] New Journal of Chemistry, 2016, vol. 40, # 8, p. 6970 - 6976 [11] Applied Catalysis A: General, 2014, vol. 475, p. 140 - 146 [12] Asian Journal of Chemistry, 2012, vol. 24, # 2, p. 653 - 656 [13] Angewandte Chemie - International Edition, 2017, vol. 56, # 28, p. 8125 - 8129 [14] Angew. Chem., 2017, vol. 129, # 28, p. 8237 - 8241,5 [15] Tetrahedron Letters, 2017, vol. 58, # 24, p. 2360 - 2365 [16] Tetrahedron Letters, 2004, vol. 45, # 15, p. 3055 - 3058 [17] Green Chemistry, 2009, vol. 11, # 6, p. 863 - 867 [18] Journal of Materials Chemistry A, 2014, vol. 2, # 33, p. 13422 - 13430 [19] Zeitschrift fur Naturforschung - Section B Journal of Chemical Sciences, 2014, vol. 69, # 5, p. 509 - 518 [20] Synthetic Communications, 2018, vol. 48, # 9, p. 1060 - 1067 [21] Turkish Journal of Chemistry, 2014, vol. 38, # 4, p. 650 - 660 [22] Tetrahedron Letters, 1992, vol. 33, # 49, p. 7535 - 7538 [23] Chemistry Letters, 2000, # 9, p. 998 - 999 [24] Organic Letters, 2018, vol. 20, # 7, p. 1970 - 1973 [25] Russian Journal of Organic Chemistry, 2000, vol. 36, # 12, p. 1703 - 1708 [26] Catalysis Letters, 2017, vol. 147, # 1, p. 167 - 180 [27] Angewandte Chemie - International Edition, 2016, vol. 55, # 51, p. 15792 - 15796 [28] Angew. Chem., 2016, vol. 128, # 51, p. 16024 - 16028,5 [29] Journal of the American Chemical Society, 1989, vol. 111, # 15, p. 5954 - 5955 [30] Journal of the American Chemical Society, 1995, vol. 117, # 50, p. 12436 - 12451 [31] Tetrahedron Letters, 2004, vol. 45, # 39, p. 7291 - 7295 [32] Synthetic Communications, 2006, vol. 36, # 22, p. 3441 - 3445 [33] Organic Preparations and Procedures International, 2007, vol. 39, # 1, p. 71 - 75 [34] Zeitschrift fur Naturforschung - Section B Journal of Chemical Sciences, 1999, vol. 54, # 4, p. 541 - 543 [35] Synthesis, 1980, # 4, p. 296 - 299 [36] Organic Letters, 2013, vol. 15, # 20, p. 5298 - 5301 [37] Tetrahedron Letters, 1996, vol. 37, # 7, p. 1113 - 1116 [38] Russian Journal of General Chemistry, 2017, vol. 87, # 10, p. 2477 - 2480 [39] Zh. Obshch. Khim., 2017, vol. 87, # 10, p. 1728 - 1731,4 [40] Bulletin of the Chemical Society of Japan, 1983, vol. 56, # 6, p. 1885 - 1886 [41] Journal of Organic Chemistry, 1984, vol. 49, # 26, p. 5195 - 5197 [42] RSC Advances, 2015, vol. 5, # 99, p. 81415 - 81428 [43] Indian Journal of Chemistry - Section B Organic and Medicinal Chemistry, 2001, vol. 40, # 5, p. 391 - 393 [44] Journal of Heterocyclic Chemistry, 2014, vol. 51, # 6, p. 1785 - 1790 [45] Journal of the American Chemical Society, 1941, vol. 63, p. 733 [46] Canadian Journal of Chemistry, 1963, vol. 41, p. 2905 [47] Tetrahedron, 1974, vol. 30, # 16, p. 2949 - 2959 [48] Journal of Organic Chemistry, 1966, vol. 31, p. 2784 - 2789 [49] Journal of Organic Chemistry, 1961, vol. 26, p. 4874 - 4878 [50] Journal of Organic Chemistry, 1967, vol. 32, p. 2372 - 2375 [51] Sov. Prog. Chem. (Engl. Transl.), 1975, vol. 41, # 7, p. 85 - 86 [52] Ukrainskii Khimicheskii Zhurnal (Russian Edition), 1975, vol. 41, # 7, p. 762 - 764 [53] Phosphorus, Sulfur and Silicon and the Related Elements, 1993, vol. 82, # 1-4, p. 91 - 98 [54] Chemical Communications (Cambridge, United Kingdom), 1998, # 9, p. 1033 - 1034 [55] Journal of the American Chemical Society, 2003, vol. 125, # 38, p. 11460 - 11461 [56] Synthetic Communications, 2004, vol. 34, # 20, p. 3801 - 3806 [57] Synthesis, 2005, # 4, p. 543 - 546 [58] Chemistry - A European Journal, 2006, vol. 12, # 32, p. 8228 - 8239 [59] Organic and Biomolecular Chemistry, 2006, vol. 4, # 9, p. 1641 - 1646 [60] Journal of Heterocyclic Chemistry, 2008, vol. 45, # 3, p. 853 - 857 [61] European Journal of Organic Chemistry, 2008, # 6, p. 975 - 993 [62] Tetrahedron Letters, 2009, vol. 50, # 34, p. 4833 - 4837 [63] Green Chemistry, 2009, vol. 11, # 4, p. 526 - 530 [64] Chemical Communications, 2011, vol. 47, # 7, p. 2053 - 2055 [65] Synthetic Communications, 2011, vol. 41, # 10, p. 1410 - 1420 [66] Catalysis Communications, 2011, vol. 12, # 13, p. 1212 - 1217 [67] Patent: US2012/122888, 2012, A1. Location in patent: Page/Page column 45 [68] Chemistry - An Asian Journal, 2013, vol. 8, # 10, p. 2459 - 2465 [69] RSC Advances, 2014, vol. 4, # 13, p. 6447 - 6453 [70] Australian Journal of Chemistry, 2013, vol. 66, # 8, p. 913 - 920 [71] European Journal of Medicinal Chemistry, 2014, vol. 85, p. 450 - 457 [72] Journal of Molecular Catalysis B: Enzymatic, 2014, vol. 109, p. 170 - 177 [73] Journal of Catalysis, 2014, vol. 317, p. 1 - 10 [74] Chemical Science, 2014, vol. 5, # 11, p. 4517 - 4524 [75] Catalysis Communications, 2015, vol. 68, p. 25 - 30 [76] Research on Chemical Intermediates, 2015, vol. 41, # 6, p. 3389 - 3400 [77] European Journal of Inorganic Chemistry, 2015, vol. 2015, # 28, p. 4699 - 4707 [78] Chemistry - A European Journal, 2015, vol. 21, # 42, p. 14862 - 14870 [79] Organic Letters, 2016, vol. 18, # 3, p. 428 - 431 [80] Angewandte Chemie - International Edition, 2016, vol. 55, # 31, p. 9060 - 9064 [81] Angew. Chem., 2016, vol. 128, p. 9206 - 9210,5 [82] Monatshefte fur Chemie, 2016, vol. 147, # 7, p. 1243 - 1249 [83] Molecules, 2016, vol. 21, # 12, [84] Polymer, 2017, vol. 112, p. 342 - 350 [85] Molecular Catalysis, 2018, vol. 453, p. 93 - 99 [86] Green Chemistry, 2018, vol. 20, # 23, p. 5336 - 5345 以环己酮和丙二腈为原料合成2-环己基亚己基丙二腈的一般步骤如下：在搅拌条件下，将1毫摩尔环己酮（羰基化合物）和1毫摩尔丙二腈（活化甲醇）溶于5毫升溶剂（二甲基甲酰胺（DMF）或乙腈（MeCN））中。加入0.0035克'HDT-F'催化剂（如实施例1所述制备）。反应进程通过薄层色谱法（TLC）监测。反应完成后，过滤去除催化剂，滤液用水洗涤，产物用硫酸钠干燥后，在减压条件下浓缩。产率基于反应过程中消耗的环己酮量，通过核磁共振（NMR）光谱分析最终产物确定。 参考文献：[1] Patent: US2005/250963, 2005, A1. Location in patent: Page/Page column 5 [2] Green Chemistry, 2010, vol. 12, # 3, p. 514 - 517 [3] Synlett, 2000, # 7, p. 1016 - 1018 [4] Collection of Czechoslovak Chemical Communications, 2005, vol. 70, # 10, p. 1727 - 1736 [5] European Journal of Organic Chemistry, 2008, # 28, p. 4763 - 4768