Lab 4: Synthesis of BF3•Me3N in a Vacuum

Equipment:

• Vacuum rack ("Schlenk line") in A105
• Bruker 500 MHz NMR
• Thermo-Nicolet FT200 FT-IR with ATR head
• melting point apparatus

Handouts:

• R.J. Angelici, Expt 19: (CH₃)₃N:BF₃, Synthesis and Technique in Inorganic Chemistry, 2nd ed, W. B. Saunders: Philadelphia, 1977, pp. 188-97.
• D.P. Shoemaker, C.W. Garland,& J.W. Nibler, Chap 27: Vacuum techniques, Experiments in Physical Chemistry , 5th ed, McGraw-Hill, NY, 1989, pp 677-714.

References:

• J.M. Miller and M. Onyszchuk, The relative acceptor power of boron trihalides and borane toward trimethylamine by proton N.M.R. measurements. Can. J. Chem. 42: 1518-23 (1964).
• B Benton-Jones, MEA Davidson, JS Hartman, JJ Klassen & JM Miller: Trimethylamine and 4-methylpyridine adducts of the mixed trihalides of boron: Exchange reactions and nuclear magnetic resonance spectra. J. Chem. Soc. Dalton, 2603-7, 1972.
• MJ Bula, DE Hamilton & JS Hartman: Donor-acceptor adducts of the mixed boron trihalides: Adducts of dimethyl ether. J. Chem. Soc. Dalton, 1405-12, 1972.
• MJ Bula & JS Hartman: Boron trihalide adducts of dimethyl sulphide. A nuclear magnetic resonance study of exchange reactions and mixed boron trihalide adducts. J. Chem. Soc. Dalton, 1047-54, 1973.
• AR Katritzky: Infrared absorption of heteroaromatic and benzenoid six-membered monocyclic nuclei. Part VI. Pyridine-boron complexes. J. Chem. Soc., 2049-2051, 1959.
• R.L. Amster & R.C. Taylor, Spectrochim. Acta 20A: 1487-1502 (1964).
• K. Nakamoto, Infrared Spectra of Inorganic and Coordination Compounds. John Wiley: New York, 1963.

Lab description:

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Diagram of the vacuum line: