関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | But-2-enamide | HCID 31877 | — |
| 反応物 | 4-(Trifluoromethyl)phenylboronic acid | HCID 2734389 | — |
| 触媒 | ethene;(Z)-4-hydroxypent-3-en-2-one;rhodium | HCID 11010647 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (R)-3-(4-Trifluoromethylphenyl)-butyramide | HCID 44236521 | — |
反応手順
Acetylacetonatobis(ethylene)rhodium(I) (0.3 mmol), (S)-(−)-2,2′-Bis(diphenyl-phosphino)-1,1′-binaphthalene (0.045 mmol), 4-(trifluoromethyl)phenylboronic acid (2 mmol), K2CO3 (0.5 mmol), and but-2-enoic acid amide (1 mmol) are added into a 25-mL round-bottomed flask containing a magnetic stirrer bar, a septum inlet, and a reflux condenser. The flask is flashed with argon and then charged with 1,4-dioxane (3 mL) and de-ionized H2O (0.5 mL). The reaction mixture is stirred for 16 hours at 100° C. The (R)-3-(4-trifluoromethylphenyl)butyramide is extracted with ethyl acetate, washed with brine, and dried over anhydrous magnesium sulfate. Chromatography over silica gel gives the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09206143B2 |
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| 出典データセット | uspto-grants-2015_12 |
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| ORD ID | ord-fd2ea75ce6ea438a88c7d78b862d7e25 |
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| 出典メモ | uspto-grants-2015_12 |
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