関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-(Trifluoromethyl)benzoyl chloride | HCID 75257 | — |
| 反応物 | Methylamine tetrahydrofuran | HCID 66615946 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-Methyl-3-(trifluoromethyl)benzamide | HCID 1490147 | — |
反応手順
A 2M methylamine-THF solution (20 ml) was added to a solution of triethylamine (7 ml) in dichloromethane (70 ml), a solution of 3-(trifluoromethyl)benzoyl chloride (5.0 g) in dichloromethane (30 ml) was added dropwise thereto under ice cooling, followed by stirring at room temperature for 72 hours. The reaction solution was poured into water, followed by extraction with chloroform. The organic layer was washed with saturated aqueous sodium bicarbonate solution and then saturated brine in this order and dried over anhydrous magnesium sulfate, and the solvent was then evaporated under reduced pressure. The residue was dissolved again in ethyl acetate, washed with saturated aqueous sodium bicarbonate solution and then saturated brine in this order, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The resulting solid was washed with diisopropylether, to obtain, as a colorless solid, N-methyl-3-(trifluoromethyl)benzamide (1.34 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08377923B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-74200f13a85849c9a1e20e868422464d |
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| 出典メモ | uspto-grants-2013_02 |
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