関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acrylic Acid | HCID 6581 | — |
| 反応物 | Phenothiazine | HCID 7108 | — |
| 反応物 | Diethylene Glycol Monobutyl Ether | HCID 8177 | — |
| 反応物 | 1-Butanesulfonamide, N-[3-(dimethylamino)propyl]-1,1,2,2,3,3,4,4,4-nonafluoro- | HCID 110558 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-[3-(Dimethylamino)propyl]-N-[(nonafluorobutyl)sulfonyl]-beta-alanine | HCID 15251601 | — |
反応手順
An acrylic acid Michael addition reaction was then run according to the general procedure given in U.S. Pat. No. 5,144,069 (Stern et al.). 50 g (0.12 mole) of the purified C4F9SO2N(H)C3H6N(CH3)2, 16.4 g (0.23 mole) of acrylic acid and 0.2 g of phenothiazine (free radical polymerization inhibitor) were added to a 250-mL three-neck flask equipped with an air stirrer and thermometer. The resulting mixture was heated to 125° C. and was allowed to react for 6 hours. After this reaction period, a positive solubility check of the product in water of pH 7 indicated that the Michael addition reaction was essentially complete. While still mixing, a solvent blend of 18 g of diethylene glycol monobutyl ether and 42 g of deionized water was added and the mixture was allowed to cool to room temperature. The water solubility test was run again with the same positive result, showing good conversion to the desired Michael addition product, C4F9SO2N(C2H4COOH)C3H6 (CH3)2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05468353 |
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| 出典データセット | uspto-grants-1995_11 |
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| ORD ID | ord-6db07f2762984316b90d6f5c14a17a70 |
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| 出典メモ | uspto-grants-1995_11 |
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