📜Biphenyl-2,2'-Diyl-Bis-Lithium置于三氯化磷体系中,用 四氢呋喃 作为反应溶剂,以69%的收率获得产物5-氯-5H-二苯并磷杂环戊二烯
参考文献:Synthesis And Structural Characterization Of A Tetraaryldiphosphorus Cation And A Dialkylphosphonium Salt
标题:Synthesis And Structural Characterization Of A Tetraaryldiphosphorus Cation And A Dialkylphosphonium Salt
摘要:The Compound 5-Chorodibenzophosphole Reacts With An Equivalent Amount Or An Excess Of Al2Cl6 In Methylene Chloride Solution To Afford The Respective Tetraorganodiphosphorus Cations [r(2)P(Cl)Pr(2)][alcl4] (R(2) = O,O'-Dibenzophenylato),1. However,Reaction Of T-Bu(2)Pcl With An Equivalent Amount Or An Excess Of Al2Cl6 In Ch2Cl2 Gives Rise To A Phosphonium Ion,[t-Bu(2)Pcl(2)][alcl4] (2) As The Major Product,While Reaction With 0.5 Equivalent Al2Cl6 Leads To A Mixture Of Cationic Organophosphorus Species. In Addition,The Compound 5-Chloro-Bis-Carboranylphosphole (3) Was Synthesized. Compound 3 Fails To React With Al2Cl6 Or Gacl3,Yet Does Afford 5-Fluoro-Bis-Carboranylphosphole (4) Upon Treatment With Agsbf6. The Molecular Structures Of 1 And 2 Have Been Determined From X-Ray Structural Analysis. The Former Consists Of A Planar P(Iii) Heterocyclic Moiety Joined To An Essentially Tetrahedral P(Tv) Heterocycle By A Single P-P Bond. The Charge Is Balanced By The Heptachlorodialuminate Ion. Compound 1 Crystallized In The Triclinic Space Group With A = 10.5798(8) Angstrom,B = 11.3656(9) Angstrom,= 13.8190(11) Angstrom,Alpha = 107.985(3)Degrees,Beta = 100.9135(2)Degrees,Gamma = 103.636(2)Degrees,V = 1478 Angstrom(3),Z = 2,R = 0.047. Compound 2 Crystallized In The Monoclinic Space Group,P2(1) With A = 7.2471(8) Angstrom,B = 12.0235(12) Angstrom,C = 9.9651(11) Angstrom,Beta = 90.473(3)Degrees,V = 868 Angstrom(3) Z = 2,R = 0.109.
DOI:10.1080/10426509608037969