McMaster University - Chem3D03 Lab Manual

Unknowns

Each student will receive samples of two unknown compounds. These are to be identified before the end of term. The two unknowns differ considerably in difficulty.

Unknown #1 is the easier of the two, and is to be solved using the Chemistry 3D03 laboratory facilities; i.e.,

m.p. or b.p.
90 MHz 1H nmr spectroscopy
infrared spectroscopy
uv/vis absorption spectroscopy
characterization of a derivative

The preparation and characterization (by melting point) of a solid derivative is to be used for verification of the structure of the unknown. The use of higher field 1H or 13C nmr spectroscopy or mass spectrometry to aid in the identification of these compounds is not permitted.

Unknown #2 is more challenging, and will be handed out in smaller quantities (~60 mg). Each student in the course will be assigned to a 4th year undergrad or graduate student in the Department, who will measure the high-field 1H and 13C nmr spectra of the compound, using a sample prepared by the student. Students are expected to be present during the recording of these spectra. The sample will then be submitted to the Departmental Mass Spectrometry facility for determination of the mass spectrum. The compound should be solvable on the basis of these data.

The unknowns are to be identified in a short report submitted to the T.A.. The report is to include copies of all spectral data, and a short written section interpreting the spectra and explaining the logic employed to solve the structures.


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Chem3D03 Lab Manual.

04feb97; wjl