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33751560853
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Aicher, T. D.; Chen, Z.; Chen, Y.; Faul, M. M.; Krushinski, J. H., Jr.; Le Huerou, Y.; Pineiro-Nunez, M. M.; Rocco, V. P.; Ruley, K. M.; Schaus, J. M.; Thompson, D. C.; Tupper, D. E. PCT Int. Appl., WO03082877, 2003.
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26
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33751579199
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note
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2), 170.7 (CO) ppm.
-
-
-
-
27
-
-
33751577236
-
-
note
-
2+ (5%).
-
-
-
-
29
-
-
33751583546
-
-
note
-
+.
-
-
-
-
30
-
-
33751564140
-
-
note
-
13C NMR spectra of the expected product 18 obtained later from Route B proved to be identical to these ones. Moreover, the m/z 489 signal corresponding to the di-N-alkylated product was also present, but in lesser abundance (<5%), in the low-resolution mass spectrum of product 18 obtained from Route B. These results led us to conclude that, at least, a part of the m/z 489 signal may result from a fragmentation process during the mass spectrometric analysis. In this case, a prolonged reaction with other portions of alkylating agent and base would probably have led to the tri-N-alkylated product 18 exclusively.
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-
-
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31
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33751559083
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note
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By using a 2-fold excess of alkylating agent, the reaction was rendered regioselective as the mono-N-alkylated product 21 was isolated in 88% yield.
-
-
-
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33
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0034935554
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Nihei K.-I., Kato M.J., Yamane T., Palma M.S., and Konno K. Synlett (2001) 1167-1169
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34
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33751558869
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note
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+ (97%).
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35
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33751555963
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Nachman, I.; Port, M.; Raynal, I.; Rousseaux, O. PCT Int. Appl., WO03074523, 2003.
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37
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