참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | (4-Fluoro-2-(1H-1,2,4-triazol-1-yl)phenyl)methanamine hydrochloride | HCID 21069882 | — |
| 촉매 | Palladium | HCID 23938 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 4-fluoro-2-(1H-1,2,4-triazol-1-yl)benzonitrile | HCID 21069880 | 99% |
반응 단계
(4-Fluoro-2-(1H-1,2,4-triazol-1-yl)phenyl)methanamine hydrochloride): Intermediate 1,4-fluoro-2-(1H-1,2,4-triazol-1-yl)benzonitrile, (2.46 g, 13.13 mmol) was dissolved in hot ethanol (150 mL). Aqueous 1N HCl (15 mL) was added followed by 10% Pd/C (200 mg). The mixture was shaken under H2 (55 psi) for 4 h., then filtered through Celite and concentrated in vacuo. The remaining residue was partitioned between ethyl acetate and water. The aqueous layer was isolated and lyophilized to give the title compound as a white powder (2.96 g, 99% yield). 1H NMR (500 MHz, CD3OD) δ ppm: 9.51 (1H, s), 8.63 (1H, s), 7.85 (1H, dd, J=8.5, 5.8 Hz), 7.68 (1H, dd, J=8.8, 2.4 Hz), 7.49 (1H, td, J=8.3, 2.4 Hz), 4.20 (2H, s). LCMS (M+H) calcd for C9H10N4F: 193.08; found: 193.16.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07173022B2 |
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| 출처 데이터셋 | uspto-grants-2007_02 |
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| ORD ID | ord-0cc37b0f01c14e7797475ffa60949e5f |
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| 출처 메모 | uspto-grants-2007_02 |
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