Separations of Threo-Erythro Aminoalcohols by Preparative HPLC

References

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• Deactivation of the “Prep-Pak”® cartridge was accomplished using diethyl or triethylamine. Aqueous ammonium hydroxide dissolves the silica gel and shortens the column life
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• No systematic study to optimize the recovery has been attempted. Several parameters such as activity of the silica gel, concentration of the diethylamine, etc. could effect the total recovery
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• A three-way valve which can be placed between the syringe and the needle is available from Popper and Sons, Newhyde Park, New York, N.Y. (Part No. 6017)
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• For the analytical LC, the solvents were filtered through a 0.45 μM millipore filter and degassed by a steady stream of helium
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• See Reference la.
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• The threo-erythro compounds shown in Table V Reference la were studied in cooperation with Dr. S. Hurlbert using 100 MHz NMR to determine the NMR shifts
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• The TLC plates used were purchased from MC/B Manufacturing and were silica gel 60 F254 on aluminum support. Layer thickness was 0.2 mm. The ammonia atmosphere was accomplished by placing a beaker of concentrated aqueous ammonia in the TLC chamber and lining the walls of the chamber with filter paper
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• The Δ Rf value can be corelated to the load which can be separated by one Prep-Pak® cartridge on a single pass through the column
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• The negative deflection could possibly be due to some soluent carried over from the preparation of the aminoalcohols or from displacement of the amine modifier, diethylamine, by the aminoalcohols
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