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71649112004
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note
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13C NMR spectroscopy.
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44
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71649097375
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note
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Preparation of cellulose or starch sulfuric acid: To a magnetically stirred mixture of 5.00 g of cellulose (DEAE for column chromatography, Merck) or starch 5.00 g (Merck) in 20 ml of n-hexane, 1.0 g of chlorosulfonic acid (9 mmol) was added dropwise at 0 °C over 2 h. HCl gas was removed from the reaction vessel immediately. After the addition was complete, the mixture was stirred for 2 h. Then, the mixture was filtered, washed with 30 ml of acetonitrile, and dried at room temperature to obtain 5.47 g cellulose sulfuric acid as a white powder or 5.06 g starch sulfuric acid as a cream powder.
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45
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71649110635
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note
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3): δ 20.73, 28.86, 29.45, 30.17, 41.65, 52.55, 62.65, 65.87, 76.14, 115.24, 120.74, 127.74, 129.81, 131.33, 142.77.
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