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Small amounts of mono-and of trisubstituted products were detected in the reaction mixtures by HPLC. The isomeric disubstituted products could not be separated by column diromatography. The use of more than 2 equiv. of BuLi and electrophile still yields a reaction mixture with isomeric disubstituted compounds as the major products. However, substantial amounts of trisubstituted and small amounts of mono-and tetrasubstituted products were detected
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9. Small amounts of mono-and of trisubstituted products were detected in the reaction mixtures by HPLC. The isomeric disubstituted products could not be separated by column diromatography. The use of more than 2 equiv. of BuLi and electrophile still yields a reaction mixture with isomeric disubstituted compounds as the major products. However, substantial amounts of trisubstituted and small amounts of mono-and tetrasubstituted products were detected.
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34
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The less clean Raney-Nickel hydrogenation of disubstituted compounds call for longer reaction times and higher temperatures
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12. The less clean Raney-Nickel hydrogenation of disubstituted compounds call for longer reaction times and higher temperatures.
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- is achieved in high yield in a simple procedure with acetic acid anhydride and acetic acid avoid ing the toxic Cbz chloride. The amide groups may be converted into tertiary amines by borane reduction, regenerating the full coordination ability of the macrocycle
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