関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl isocyanatoacetate | HCID 76283 | — |
| 反応物 | Dihexyl 2-isocyanatobutanedioate | HCID 86656430 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | N,N-dimethylformamide; methylsulfinylmethane | HCID 3013483 | — |
| 生成物 | Dihexyl aspartate carbamate | HCID 86656429 | — |
反応手順
2.7 g (i.e., 50 mmol of hydroxyls) of dextran with a weight-average molar mass of approximately 10 kg/mol (Bachem) are dissolved in a DMF/DMSO mixture. The mixture is brought to 130° C. with stirring and 3.2 g (25 mmol) of ethyl isocyanatoacetate and then 3.9 g (8 mmol) of dihexyl 2-isocyanatobutanedioate are gradually introduced. After reacting for 1 h, the medium is diluted in water and purified by diafiltration through a 5 kD PES membrane against 0.1N NaOH, 0.9% NaCl and water. The final solution is quantitatively determined by dry extract, in order to determine the concentration of polymer. A fraction of solution is lyophilized and analyzed by 1H NMR in D2O in order to determine the degree of conversion of the hydroxyls to N-(sodium methylcarboxylate) carbamate and the degree of the functionalization of the hydroxyls to give dihexyl aspartate carbamate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09115218B2 |
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| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-17fc1b3fe5f0430aa9b1b5535a8d6449 |
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| 出典メモ | uspto-grants-2015_08 |
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