2-甲基-2-苯丙基氯化镁合成路线 (共 22 条)
反应条件
in diethyl ether; toluene 1.44M Et2O soln. of NeophMgCl (1.7-2.05 equiv.) dropwise with stirring added to toluene soln. of SnCl4 (1 equiv.) under N2 at room temp., heatedat reflux for 3 h, left at room temp. for 12 h; aq. satd. soln. NH4Cl added, organic layer separated, aq. layer extracted with Et2O, combined organic extracts dried over MgSO4, solvent removedunder vac., recrystd. from n-heptane; ratio of Nph3SnCl/Nph2SnCl2 was 6 0/40-24.5/75.5, NMR;
参考文献
Zuniga, Adriana E.; Fidelibus, Pablo M.; Mandolesi, Sandra D.; Podesta, Julio C.
Journal of Organometallic Chemistry, 2011 , vol. 696, # 8 p. 1547 - 1555
反应条件
in not given according to J. Organomet. Chem. 2011, 696, 1547;
参考文献
Gerbino, Dario C.; Scoccia, Jimena; Koll, Liliana C.; Mandolesi, Sandra D.; Podesta, Julio C.
Organometallics, 2012 , vol. 31, # 2 p. 662 - 671
反应条件
1: (2-methyl-2-phenylpropyl)MgCl With zinc(II) chloride in tetrahydrofuran 2: iodobenzene With dichloro bis(acetonitrile) palladium(II); diethyl bicyclo[2.2.1]hept-2,5-diene-2,3-dicarboxylate in tetrahydrofuran T=60°C; Negishi coupling reaction; 2 h; Inert atmosphere;
参考文献
Liu, Qiang; Duan, Hui; Luo, Xiancai; Tang, Yang; Li, Gang; Huang, Rong; Lei, Aiwen
Advanced Synthesis and Catalysis, 2008 , vol. 350, # 9 p. 1349 - 1354
反应条件
1: in diethyl ether T=-78 - 20°C; 2: With hydrogenchloride in diethyl ether; water; ethyl acetate
参考文献
MERCK and CO., INC.
Patent: WO2007/108968 A2, 2007 ;
Location in patent: Page/Page column 29-30 ;
反应条件
2-chloro-1,2-diphenyl-ethanone; zinc(II) chloride; ((S)-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl)PdCl2*2THF T=20°C;
参考文献
Lei, Aiwen; Zhang, Xumu
Organic Letters, 2002 , vol. 4, # 14 p. 2285 - 2288
反应条件
1: (2-methyl-2-phenylpropyl)MgCl With zinc(II) chloride in tetrahydrofuran T=20°C; 2: 1-tributylstannyl-2-phenylacetylene With bis(dibenzylideneacetone)-palladium(0) in dichloromethane Further stages.;
参考文献
Jin, Liqun; Zhao, Yingsheng; Wang, Haibo; Lei, Aiwen
Synthesis, 2008 , # 4 p. 649 - 654
反应条件
in diethyl ether byproducts: bineophyl; under Ar, Grignard reagent (prepared from Mg and neophylchloride), stirred under reflux (18 h), add. to GaCl3 soln. (30 min), stirred under reflux (18 h); vac. dest. at room temp., extraction from MgCl2, washed (pentane), vac. dest. at 120-210°C (160-210°C pure product), recrystn. (pentane, -20°C); elem. anal.;
参考文献
Beachley, O. T. Jr.; Noble, M. J.; Churchill, Melvyn Rowen; Lake, Charles H.
Organometallics, 1992 , vol. 11, p. 1051 - 1055
反应条件
in diethyl ether 1 h reflux;
参考文献
Gmelin Handbook: Sn: Org.Verb.1, 1.1.1.13, page 122 - 129
反应条件
in diethyl ether; benzene final reflux in benzene;
参考文献
Zimmer,H. et al.
Journal of Organic Chemistry, 1966 , vol. 31, p. 3857 - 3860
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Gmelin Handbook: Sn: Org.Verb.1, 1.1.1.13, page 122 - 129
反应条件
1: diethyl ether; benzene View Scheme
参考文献
Sn: Org.Verb.1, 1.1.1.13, page 122 - 129