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75749101272
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See Ref. 12g
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See Ref. 12g.
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75749086685
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note
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Commercially available aminopropylated glass slides were found to have lower loading levels than those required for our purpose, so we independently fabricated them by the aminopropylation of unmodified porous glass slides. Our protocol for this was based on the results of an examination of the immobilization conditions with a selection of materials. For an example of a similar aminoalkylation protocol, see Ref. 4a.
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41
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75749116998
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note
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2 (877 μl). After warming at 60 °C for 12 h, the reaction mixture was allowed to cool to room temperature and then diluted with water (10 ml). The resulting mixture was extracted with EtOAc (2 × 5 ml), and the combined organic phases were concentrated and dried in vacuo to yield a slurry (2.46 mg). The crude product was purified by reversed-phase HPLC to produce 3a (2.12 mg, 95.5% from 1) as a colorless oil.
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42
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75749119211
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note
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2 had hardly any influence.
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