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The Alkylation of the Boron Hydrides, Reaction of Pentaborane-9 with 1

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The Alkylation of the Boron Hydrides, Reaction of Pentaborane-9 with 1 This dissertation has been 62-829 microfilmed exactly as received ! ALTWICKER, Elmar Robert, 1930- j THE ALKYLATION OF THE BORON HYDRIDES; REACTION OF PENTABOlLANE-9 WITH 1-BUTENE AND SOME POLYHALOGENATED HYDROCARBONS. The Ohio State University, Ph.D., 1957 Chemistry, organic University Microfilms, Inc., Ann Arbor, Michigan THE ALKYLATION OF THE BORON HYDRIDES Reaction of Pentaborane-9 with 1-Butene and Some Polyhalogenated Hydrocarbons DISSERTATION Presented in Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in the Graduate School of The Ohio State University EIZvIAR RP'^TWIGKER, B.S. The Ohio State University 1957 Approved by; m Departme Ï Chemistry Acknowledgement The author would like to thank Professor A.B, Garrett for the supervision of this research. He would also lik e to thank Dr. John Norman of the Olin-Mathieson Chemical Corporation for the mass spectrographic analyses. 11 Table of Contents Page I. Purpose .................................................... ...... 1 II. Historical ..................... ........... 2 III, Experimental ....................................... 5 A. Apparatus ............................ ......... $ 1. Main Vacuum System .................... ... ^ 2. Reaction-, Transfer-, and Storage A pparatus............................................................ ^ 3. Analytical Apparatus .......... Vy 5. Materials l 6 G. Reaction of Pentaborane-9 with 1-Butene . 18 1. Reaction and Separation of the Reaction Mixture ............ 19 2. Identification of Butylpentaborane . 2h 3. Results .......................................................... 30 Ü. Summary .......................................................... ill D. Reaction of Pentaborane-9 with Triraethyl- borane ...... ............................ ..... k2 E. Reaction of Pentaborane-9 v/ith Ethyl Magnesium Bromide ........................................ F. Reaction of Pentaborane-9 with Solvents . U9 1. Aromatic Compounds ................ « ................... $0 2. Methyl Cyanide .................................. $ l 3. n-Heptane ....................................... i l l Table of Contents (Continued) Page G. Reaction of Pentaborane-9 vrLtb Some Polyhalogenated Hydrocarbons ....... $9 1. Introduction ........................................ $9 2. Reaction and Separation of the Reaction Mixture...... ....................................... ................... .... 6 l 3. Analysis ................. 68 U. Reaction of Pentaborane-9 with Diehloromethane, Dibromomethane, and Broraochloromethane ....... 71 a. Dichloromethane » . ............................ 73 b. Identification of 1,1’-Dipentaboiyl- methane ........... 7k c. Summary................................................... 63 d. Identification of 1-Pentaboryl- borondichloromethane ................................. 8U e. Bromochloromethane ..... 85 f. Dibromomethane ...» 87 g. Summary ................ 87 5. Reactionrof Pentaborane-9 with Chloroform . 88 6 . Reaction of Pentaborane-9 with Dichloro- bromomethane .......................................... .. 97 7. Reaction of Pentaborane-9 with Carbon Tetrachloride ....................... 103 8 . Reaction of Pentaborane-9 with 1,2-Dichloro- ethane and l-3romo-2-chloroethane ..... 105 9. a. 1,2-Dichloroethane ...................... .. 106 b. l-Bromo-2-chloroethane ..................... 110 IV. Discussion ...................................... 118 A. G e n e r a l.......................................................................... 118 B. Reaction of Pentaborane-9 vrith l-Butene .... 120 iv Table of Contents (Continued) C. Reaction of Pentaborane-9 with Polyhalogenated hydrocarbons ....................... ••••• 122 D, Reaction with Solvents .................................... , . * 132 7. Sum m ary ..................................................................................... 13U Bibliograpliy ........................................................................ 136 Autobiography ................... 138 A L is t of Tables Table Page I. Cooling baths . ........................................................... 14 II. Reaction of Pentaborane-9 with 1-butene ...... .31»32,33 I I I . Vapor pressure of 2-n-butylpentaborane-9 .......................... 30,39 IV. Reaction of Pentaborane-9 with Trimethylborane . 43 V. Reaction of Pentaborane-9 with Solvents . ..................56,57 VI. Reaction of Pentaborane-9 with Methylene Halides . ............................. 75,7&,77 VII. Reaction of Pentaborane-9 with Chloroform .......................90,91,92 VIII. Reaction of Pentaborane-9 with Dichlorobroiaomethane ............................99 IX* Reaction.of Pentaborane-9 with Carbon Tetrachloride ............................ 103 X. Reaction of Pentaborauie-9 with 1,2-Dichloroethane . ...........................106 XI. Reaction of Pentaborane-9 with l-bromo-2- chloro ethane . ................ 110 v i List of Illustrations Figure Page 1. Vacuum System .......................................................... 6 2. Section of Fractionation Train •••.» ........................ • 8 3* Reaction Vessels 10 U, Storage Tubes, Infrared Samples, and Tube Opener * • • . 12 Fractionation Scheme ••••• .................................... ••• 22 6 . Vapor Pressures of Reaction Components •• •• 23 7. Infrared Spectrum of 2-n-3utylpentaborane-9 ...... 8 . Infrared Spectrum of Pentaborane-9 ........... 35 9. Infrared Spectruin of Tri-n-Bu.tylborane (impure) ..... 37 10. Vapor Pressure of 2-n-Butylpentaborane-9 . ................. UO 11. Infrared Spectmim of Solid Reaction Product ....... 52 12. Infrared Spectrum of Solid Reaction Product ....... 5U 13. Infrared Spectrum of Mixture .............. 58 lU. Vapor Pressures of Reactants ...... ............................. 60 15. U-Trap D istilla tio n ................................. 66 16 . Transfer Arrangement ................. ..... 69 17. Sublimator.................................. ......................................... 69 18. Infrared Spectrum of 1 -Methylpentaboranc-9 . ................. 79 19. Infrared Spectrum of 1,1'-Dipentaborylmethane ...... 80 20. Vapor Pressure of 1 ,1 '-Dipentaboiylmethane ....... 82 21. Infrared Spectnua of Fraction (v.p. 11 mm/o®) ...... 86 22. Infrared Spectrum of Mixture from Run 18-120 ...... 9U 23. Infrared Spectrum of 1-PentaborylborondichD.oromethane . 96 v li List of Illustrations (Continued) Figure Page 2U. Infrai’sd Spectrum of Tars from Reaction of Pentaborane-9 with Chloroform (and AICI 3 ) in Carbon D isulfide ............................................................ 98 2S« Infrared Spectrum of Gaseous Mixture 100 26 . Infrared Spectrum of Fi’action (v.p. 2 mm/25®) • • • • 102 27. Infrared Spectrum of l-Etbylpentaborane-9 ••**.• 100 28. Infrared Spectinun of l-Ethylpentaborane-9 .•••.• 109 29. Infrared Spectrum of l-Pentaboryl-2-chloroethane . Ill 3 0. Infrared Spectrum of 0°-Trap Fraction ......................... 1])^ 31. Infrared Spectrum of -36“-Trap Fraction ....... Il5 3 2 . Pentaborane-9, Space Relationship . ...................... I I 9 33. Mechanism of Formation of l,l*-Dipentaborylmethane . 12U v i i i THE ALKXUTION OF THE BORON HIDRIDES The Reaction of Pentaborane-9 with 1-Batene and with Some Poljdialogenated Hydrocarbons I . Purpose The purpose of th is research was to study reactions vdiich would lead to alkylation of pentaborane-9. A butyl derivative, 2-n-butylpentaborane-9, was prepared by the reaction of penta- borane-9 with 1-butene, Reactions of pentaborane-9 with a number of pol^alogenated hydrocarbons were investigated with the objective of preparing compounds containing more than one pentaboryl group per molecule. In connection with the latter reactions, the reaction of pentaborane-9 with a series of solvents was also briefly studied. -1 - II. Historical Until recently, known reactions of boron hydrides with organic molecules were almost completely limited to the lowest member of the boron hydride series, diborane. Most of the reactions reported in the literature led to products resulting from breakdown of the diborane structure. Stock^ first reported on the reactions of boron hydrides. 1. A. Stock, The Hydrides of Boron and Silicon. Cornell University Press, Ithaca, New York, 1933* chiefly diborane and tetraborane, with substances such as ethane, ethylene, acetylene, and ethanol. Decomposition was invariably the main reaction. No substituted diboranes were obtained. An attendit to prepare ethyldiborane from chlorodiborane and zinc diethyl re­ sulted in the formation of a white solid which was not further identified^. The direct msthylation of diborane with zinc dimethyl 2. H. I. Sohiesinger and A. B. Burg, J. Am. Chem. Soc.. 53. 4331 (1931). ______________________________________________________ 3 supposedly led to trace amounts of methyldiboranes . 3. H. I. Schlesinger and A. 0. Walker, J. Am. Chem. Soc.. 57. 621 (1935). -2 - -3 - In the late thirties Sehlesinger and co-wrkera^*^ succeeded 4* H.8ohlesinger, L. Horvitz and A, B. Burg, J. Am. Chem. Soc.. 9B. 407 (1936). 5• ÜSehlesinger, N, W, Florin and A, B, Burg, J. Am. Chem. Soc.. 6 L 1078 (1939). in substituting up to four hydrogens in diborane by alkyl groups. The reactio n was based on the equilibrium between diborane and trialkylboranes. Reactions of diborane with saturated and un­ saturated hydrocarbons, and benzene at elevated temperatures led chiefly to trialkylboranes and polymeric products containing B-C bonds^. The main products obtained from reactions of boron 6 , D, T. Hurd, J . Ab u Obem. Soc.. ]&, 2053 (1948). ' ■ I ■ I II
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