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3I (5.5 mL, 0.088 mol) was added dropwise and then refluxed for 17 h. Volatiles were removed by vacuum evaporation, and low molecular weight components were removed by dialysis (12 h): 50% EtOH in 50 mM HCl (x3), 20% EtOH in 50 mM HCl (x3), 10% EtOH in 50 mM HCl (x3), 50 mM HCl (x3), water (x3). The Alk-PEI obtained, 10.2 g, was dried by lyophilization.
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36
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4644271293
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1H HMBC and XPS experiments show several types of tertiary and quaternary amine species, respectively. This is probably due to primary formation of such moieties by alkylation with iododecane and iodomethane and some additional formation of such moieties during the purification process (dialysis in the presence of HCl).
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