University of Vermont

CHEM 201 Advanced Chemistry Laboratory

Chem 201 Lab 4: Vacuum Synthesis

Lab 4: Synthesis of BF3•Me3N in a Vacuum

Equipment:

  • Vacuum rack ("Schlenk line") in A105
  • Agilent (Varian) 500 MHz NMR
  • Shimadzu IRAffinity-1 FT-IR spectrometer with attenuated total reflectance (ATR) head
  • melting point apparatus

Handouts:

get PDFs

  • 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:

get PDFs shown in maroon below
Papers with IR data:
  • 1. RL Amster & RC Taylor: Spectroscopic studies of Lewis acid-base complexes: I. Vibrational spectra and assignments for trimethylamine complexes of boron halides. Spectrochim. Acta 20A: 1487-1502, 1964.
  • 2. PH Laswick & RC Taylor: Spectroscopic studies of lewis acid - base complexes: IV. An infrared study of oriented single crystals and normal coordinate analyses of trimethylamine - boron halide adducts. J. Molec. Structure 34: 197-218, 1976.
  • 3. K Iijima & S Shibata: Molecular structure and internal rotation of trimethylamine-boron trifluoride. A combination of electron diffraction and spectroscopic data. Bull. Chem. Soc. Japan 52: 711-715, 1979.
Papers with NMR data:
  • 1. JM Miller & M Onyszchuk: The relative acceptor power of boron trihalides and borane toward trimethylamine by proton n.m.r. measurements. Can. J. Chem. 42: 1518-1523, 1964.
  • 2. 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 Trans. 23: 2603-2607, 1972.
  • 3. JM Miller & TRB Jones: Carbon-13 nuclear magnetic resonance studies of trimethylamine adducts of the mixed trihalides of boron. Inorg. Chem. 15: 284-287, 1976.
  • 4. A Fox, JS Hartman & RE Humphries: Mixed boron trihalide adducts of amines: a multinuclear nuclear magnetic resonance study. J. Chem. Soc. Dalton Trans. 1275-1283, 1982.

Lab description:

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Diagram of the vacuum line:

Vacuum Line Drawing

Last modified April 18 2013 05:06 PM

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