참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| 반응물 | 6-(Trifluoromethyl)nicotinic acid | HCID 2777551 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | 5-(Azidomethyl)-2-(trifluoromethyl)pyridine | HCID 86601757 | 99% |
반응 단계
Into ethyl acetate was suspended 1.91 g of 6-(trifluoromethyl)nicotinic acid, and then 1.52 g of triethylamine and 3.03 g of DPPA were added thereto, followed by 3 hours of stirring. The reaction solution was washed with a saturated sodium bicarbonate aqueous solution and saturated saline and the solvent was removed by evaporation to obtain 2.0 g of 6-(trifluoromethyl)nicotinyl azide as a solid. The resulting acid azide was dissolved into 20 ml of toluene and the solution was heated and refluxed to convert the acid azide into 5-isocyanato-2-(trifluoromethyl)pyridine. Thereafter, 1 ml of methanol was added thereto at room temperature, followed by 1 hour of stirring. The reaction solution was washed with water and then dried over anhydrous magnesium sulfate. Thereafter, the solvent was removed by evaporation to obtain 1.2 g of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07666873B2 |
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| 출처 데이터셋 | uspto-grants-2010_02 |
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| ORD ID | ord-eacacc03ab534fa1a252dbbb166d772e |
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| 출처 메모 | uspto-grants-2010_02 |
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