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85038553492
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note
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2 to 100ml, and stored at -20°C. Purity of N-H ketimine solution by GC analysis was above 90%. N-H ketimine solutions were used without further purification, except evaporation prior to use to remove excess ammonia.
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15. Studies involving reductive alkylation in solid phase manner to prepare other scaffolds were also reported, see: (a) Szardenings AK, Burkoth TS, Look GC, Campbell DA. J. Org. Chem. 1996, 61, 6720-6722.
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When the acetylation was omitted, the final product sometimes contaminated with non-alkylated hydantoin (1∼6%)
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17. When the acetylation was omitted, the final product sometimes contaminated with non-alkylated hydantoin (1∼6%).
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48
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0014772602
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18. Kaiser E, Colescott RL, Bossinger CD, Cook PI. Anal. Biochem. 1970, 34, 595-598.
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49
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85038539483
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note
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19. By-products were non-alkylated hydantoin (15%), unknown (35%), and others (25%). Unknown impurities seemed to be resulted from reaction of primary amine with TMOF, because blank experiment (same experimental procedure, only without acetophenone) showed identical unknown peak on GC chromatogram
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85038539655
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note
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3 silica gel with ethyl acetate, and evaporated to give products as white solid or oil.
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51
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85038553350
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note
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+, 11), 279 (9), 105 (100).
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