新型给电子体的合成与应用研究
摘要
研究了以芴为原料合成给电子体前体9，9-双(羟甲基)芴，对合成中的影响因素进行了分析，找到最佳反应条件。对9，9-双(羟甲基)芴再进行甲基化反应，提供了合成醚类给电子体的方法，详细比较了各种方法的差异。研究了以9，9双羟甲基芴，9-羟甲基芴合成酯类化合物的方法。通过格氏路线合成环戊基三甲氧基硅烷，对各化合物工艺条件进行了研究优化，为工业应用提供了可靠依据。
We investigated that the reaction of 9,9-bis(hydromethyl)fluorene through the material fluorene. The influence facts in reaction are discussed and the best conditions are found. With the 9,9-bis(hydromethyl)fluorene , we developed new methods to synthesis of ethers. Different synthesis methods are compared. We also studied the reactions of preparing esters. The Cyclopentyl-trimethoxy-silane (CPTMS) is synthesized by reaction of tetra-methoxy silane with cyclopentyl Grignard regents in ethyl ether solvent. The opium conditions are gathered for the available date for industrial trial
We investigated that the reaction of 9,9-bis(hydromethyl)fluorene through the material fluorene. The influence facts in reaction are discussed and the best conditions are found. With the 9,9-bis(hydromethyl)fluorene , we developed new methods to synthesis of ethers. Different synthesis methods are compared. We also studied the reactions of preparing esters. The Cyclopentyl-trimethoxy-silane (CPTMS) is synthesized by reaction of tetra-methoxy silane with cyclopentyl Grignard regents in ethyl ether solvent. The opium conditions are gathered for the available date for industrial trial
引文
[1] 产经网 中国化工报 2003．9．15
[2] 毛炳权 发展我国聚烯烃技术的一些建议 《石油炼制与化212》2001．32(12)1～5
[3] Hydroc. Proc, 2001, (8): 11
[4] Eur. Chem. News, 2000, 72(1903): 1
[5] Chem. Week, 2000, 162(33): 15
[6] Chem. Week, 2000, 162(30): 18
[7] Eur. Plast News, 1999, 26(18): 16
[8] 毛炳权等，CN85 100997 1987
[9] 毛炳权等，CN1091748A 1993
[10] 金茂筑等，CN121506A 1999
[11] 毛炳权等，第八届全国催化会议论文集，1996：41
[12] Ewen J. A, J. Am. Chem. Soc., 1988, 110:6255
[13] Ewen J. A, CN 1100733A, 1995
[14] PellecchiaC, propoA, LongoP et al. Makromaol. Chem. Rapid Commun, 1992, 13: 277.
[15] Exxon. U.S. Patent 5026798, 1991
[16] 田军，胡宁海，中国科学，1995，25：237。
[17] Exxon. U. S. Patent 5017714, 1991
[18] Suejda S. A, Brookhart M. Organometallics, 1999, 18: 65.
[19] Britovsek GJP, Gibson VC, Kimberley BS, et al. Chem. Commun, 1998, 849.
[20] Small BL, Brookhart M, Bennett AMA, J.Am. Chem. Soc., 1998, 120: 4049.
[21] Chemical and Engineering Information, April, 13, 1998.
[22] Pellecchia C, Mazzeo M, PapPalardo D. Macromol Rapid Commun, 1998, 19:651.
[23] 金茂筑，快报(中国化工信息中心，原化工部经济技术委员会)68，1995。
[24] Montedision. British Patent 1286 867, 1968.
[25] 胡友良，高分子通报，1999(3)，21
[26] 钟赤锋等，高分子学报，2003(2)，266。
[27] 洪定一主编，聚丙烯原理技术，2003，39。
[28] MoroiniG etal. Macromolecules, 2001, 33: 8953.
[29] BarinoL, Scordamaglia R. Macromol Theory Simal, 1998, 7, 407.
[30] BusicoV, CipulloR, Chadwick etal. Macromolecules, 1999, 32: 4173.
[31] Barbe P. C, Gecchin G, NoristL. Adv. Polym. Sci, 1986, 81: 1.
[32] Himont Incorporated, U. S. Patent 4971937, 1990.
[33] AlbizzatiE, GianniniU, etal. Ziegler Catalysts, 1995:413.
[34] 徐君庭，封麟先，王森辉等，浙江大学学报(自然科学版)，1998，32，3：32
[35] 徐德民，韩世敏，胡友良等，化学通报，2000(7)：8
[36] Sacchi MC,Tritto I,Locatelli P. Prog Polymer Science,1987,81:1-81
[37] Barino L, Scordamaglia R. Macromol.Theory Simul. 1998,7:101-111
[38] Scordamaglia R,Barino L. Macromol.Theory Simul. 1998,7:399-405
[39] Eugene WesslenB. Acta chem. Sccind., 1967, 21:718-72
[40] SecchinG. Polypropylene Past, Present and Future The challenge Continue, 1998.
[41] MoriniG, Enrico Albizzati, Les Mingozzi. Macromolecules, 1996, 29, 5770.
[42] AlbizzatiE, GalimbertiM, Gianninill, et al. Macromol, Symp, 1995, 89: 73.
[43] 聂新水等，中国医药工业杂志，1993，24(4)：147。
[44] Kubota T, Yamamoto A,Endo M, et al. Preparation of Organoalkoxysilanes by Grignard reaction, JP: 06-345781, 1994.
[45] Ueki S, Ookura M, Ishihara T, et al. Preparation of Cyclopentyl-2-pentoxyd-imethoxysilane. JP: 07-206876, 1995.
[46] Sato R, Ueki S, Aoki T, et al. Cyclopentyl Silane compound, its preparation. EP: 486116, 1992
[47] NattaG, Corradini P, Allegra G.. J.Polym.Sci., 1961,51:387
[48] NattaG. Chim.Ind.(Milano), 1960,42(11): 1207
[49] BusicoV, CipulloR. J. Am. Chem. Soc., 1994, 116:9329
[2] 毛炳权 发展我国聚烯烃技术的一些建议 《石油炼制与化212》2001．32(12)1～5
[3] Hydroc. Proc, 2001, (8): 11
[4] Eur. Chem. News, 2000, 72(1903): 1
[5] Chem. Week, 2000, 162(33): 15
[6] Chem. Week, 2000, 162(30): 18
[7] Eur. Plast News, 1999, 26(18): 16
[8] 毛炳权等，CN85 100997 1987
[9] 毛炳权等，CN1091748A 1993
[10] 金茂筑等，CN121506A 1999
[11] 毛炳权等，第八届全国催化会议论文集，1996：41
[12] Ewen J. A, J. Am. Chem. Soc., 1988, 110:6255
[13] Ewen J. A, CN 1100733A, 1995
[14] PellecchiaC, propoA, LongoP et al. Makromaol. Chem. Rapid Commun, 1992, 13: 277.
[15] Exxon. U.S. Patent 5026798, 1991
[16] 田军，胡宁海，中国科学，1995，25：237。
[17] Exxon. U. S. Patent 5017714, 1991
[18] Suejda S. A, Brookhart M. Organometallics, 1999, 18: 65.
[19] Britovsek GJP, Gibson VC, Kimberley BS, et al. Chem. Commun, 1998, 849.
[20] Small BL, Brookhart M, Bennett AMA, J.Am. Chem. Soc., 1998, 120: 4049.
[21] Chemical and Engineering Information, April, 13, 1998.
[22] Pellecchia C, Mazzeo M, PapPalardo D. Macromol Rapid Commun, 1998, 19:651.
[23] 金茂筑，快报(中国化工信息中心，原化工部经济技术委员会)68，1995。
[24] Montedision. British Patent 1286 867, 1968.
[25] 胡友良，高分子通报，1999(3)，21
[26] 钟赤锋等，高分子学报，2003(2)，266。
[27] 洪定一主编，聚丙烯原理技术，2003，39。
[28] MoroiniG etal. Macromolecules, 2001, 33: 8953.
[29] BarinoL, Scordamaglia R. Macromol Theory Simal, 1998, 7, 407.
[30] BusicoV, CipulloR, Chadwick etal. Macromolecules, 1999, 32: 4173.
[31] Barbe P. C, Gecchin G, NoristL. Adv. Polym. Sci, 1986, 81: 1.
[32] Himont Incorporated, U. S. Patent 4971937, 1990.
[33] AlbizzatiE, GianniniU, etal. Ziegler Catalysts, 1995:413.
[34] 徐君庭，封麟先，王森辉等，浙江大学学报(自然科学版)，1998，32，3：32
[35] 徐德民，韩世敏，胡友良等，化学通报，2000(7)：8
[36] Sacchi MC,Tritto I,Locatelli P. Prog Polymer Science,1987,81:1-81
[37] Barino L, Scordamaglia R. Macromol.Theory Simul. 1998,7:101-111
[38] Scordamaglia R,Barino L. Macromol.Theory Simul. 1998,7:399-405
[39] Eugene WesslenB. Acta chem. Sccind., 1967, 21:718-72
[40] SecchinG. Polypropylene Past, Present and Future The challenge Continue, 1998.
[41] MoriniG, Enrico Albizzati, Les Mingozzi. Macromolecules, 1996, 29, 5770.
[42] AlbizzatiE, GalimbertiM, Gianninill, et al. Macromol, Symp, 1995, 89: 73.
[43] 聂新水等，中国医药工业杂志，1993，24(4)：147。
[44] Kubota T, Yamamoto A,Endo M, et al. Preparation of Organoalkoxysilanes by Grignard reaction, JP: 06-345781, 1994.
[45] Ueki S, Ookura M, Ishihara T, et al. Preparation of Cyclopentyl-2-pentoxyd-imethoxysilane. JP: 07-206876, 1995.
[46] Sato R, Ueki S, Aoki T, et al. Cyclopentyl Silane compound, its preparation. EP: 486116, 1992
[47] NattaG, Corradini P, Allegra G.. J.Polym.Sci., 1961,51:387
[48] NattaG. Chim.Ind.(Milano), 1960,42(11): 1207
[49] BusicoV, CipulloR. J. Am. Chem. Soc., 1994, 116:9329