참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 3-(Trifluoromethyl)benzoyl chloride | HCID 75257 | — |
| 반응물 | Methylamine tetrahydrofuran | HCID 66615946 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | N-Methyl-3-(trifluoromethyl)benzamide | HCID 1490147 | — |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08377923B2 |
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| 출처 데이터셋 | uspto-grants-2013_02 |
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| ORD ID | ord-74200f13a85849c9a1e20e868422464d |
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| 출처 메모 | uspto-grants-2013_02 |
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