참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 반응물 | 4-Fluoro-2-(trifluoromethyl)benzoic acid | HCID 688255 | — |
| 반응물 | Methylamine tetrahydrofuran | HCID 66615946 | — |
| 촉매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-fluoro-N-methyl-2-(trifluoromethyl)benzamide | HCID 22095075 | — |
반응 단계
DMF (3 drops) and oxalyl chloride (2.55 ml) were added to a mixture of 4-fluoro-2-(trifluoromethyl)benzoic acid (5.50 g) and dichloromethane (50 ml), followed by stirring at room temperature for 3 hours. The reaction solution was added dropwise to a 2M methylamine-THF solution (17.3 ml) and a solution of triethylamine (5.55 ml) in dichloromethane (50 ml) under ice cooling, followed by stirring for 30 minutes and concentration under reduced pressure, addition of water and extraction with ethyl acetate. The organic layer was washed with water, 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 residue was washed with diisopropylether to obtain 4-fluoro-N-methyl-2-(trifluoromethyl)benzamide (4.37 g) as a white solid.
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-d0fb158523c248fca59354d4fe3383c2 |
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| 출처 메모 | uspto-grants-2013_02 |
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