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Water → 2-(Butyl-ethyl-amino)-5-trifluoromethyl-benzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Butylethylamine | HCID 25914 | — |
| 反応物 | 2-Fluoro-5-(trifluoromethyl)benzaldehyde | HCID 2734904 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-(Butyl-ethyl-amino)-5-trifluoromethyl-benzaldehyde | HCID 86626752 | 91.9% |
反応手順
2-Fluoro-5-trifluoromethyl-benzaldehyde (5.0 g) and butyl-ethyl-amine (3.95 g) are dissolved in toluene (50 ml) and thereto is added potassium carbonate (10.78 g) and the mixture is heated under reflux overnight. The reaction solution is cooled to room temperature, and thereto are added water and diethyl ether, and the mixture is separated, and the organic layer is washed with a saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The resulting residue is purified by silica gel column chromatography (hexane:ethyl acetate=19:1→4:1) to give 2-(butyl-ethyl-amino)-5-trifluoromethyl-benzaldehyde (6.54 g). MS (m/z): 274 [M+H]+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07906517B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-8797808e003843358f9208d04ccbea49 |
| 出典メモ | uspto-grants-2011_03 |