Investigation of Factors Influencing the Stereochemistry of the Wittig Reaction
Investigation of Factors Influencing the Stereochemistry of the Wittig Reaction
Kresse, Jerome Thomas
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of cyclohexene the internal standard is added. The mixture is then either analyzed immediately by v. p. c. or the receiver is kept in a Dry Ice and acetone bath until the analysis is performed. Analysis The analyses were all run on the F and M Model 700 using a 25 ft. x 1/4 in. O.D. column containing 10 per cent by weight of J3, g^-oxydipropionitrile on 60-80 mesh Chromosorb P. The column temperature was 25° t 1° C. and the flow rate approximately 75 ml. per minute. The size of the sample injec...ted was 0.3 p-l. Calibration of the Internal Standard A series of synthetic mixtures containing known amounts of trans -1,3- pentadiene and cyclohexene, the internal standard, were prepared in tetrahydro- furan in concentrations such that the sensitivity setting of the chromatograph would be the same or very close to those used during the actual runs. The samples were made up by volume at 20° C. For example, the "known" containing 50 mole per cent 1, 3-pentadiene was prepared in the following way.
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