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Galactosyl azide 5 was synthesized according to standard procedures (three steps from D-galactose via the pentaacetate and the 1-azido tetraacetate). See, for example: a) Z. Györgydéak, L. Szilàgyi, Liebigs Ann. Chem. 1987, 235-241;
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note
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The loading was determined by elemental analysis and found to be reproducible. It should be noted that the loading calculated from the nitrogen content was in good agreement with the loading calculated either from complete fluoridolytic cleavage of 11a and isolation of 8 or from hypothetical quantitative coupling of 8 with 10a.
-
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68
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4644239222
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note
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-1, the resin mass stemming from the carbohydrate unit is 19 mg (corresponding to 38%).
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The loading of resin 2a was calculated from the nitrogen content of an aliquot of 2a being thoroughly washed and dried in vacuo at 40°°C (see also ref. [23]).
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75
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4644247474
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note
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Purification includes evaporation of the combined wash solutions, filtration over a short pad of silica, and elution of the crude product with petroleum ether/ethyl acetate (1:1).
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76
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4644243986
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note
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1H NMR data with compounds of known configuration that were synthesized by analogous routes.[14b]
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77
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The diastereomeric ratio for 18q obtained from treatment of resin 17q with TBAF was found to be equal to the one determined after cleavage with HF-pyridine.
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