참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate | HCID 151348 | — |
| 반응물 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 반응물 | 2-(4'-Fluorobiphenyl-4-yl)-2-phenylacetic acid | HCID 57779683 | — |
| 용매 | Pyridine | HCID 1049 | — |
| 생성물 | 2-(4'-fluorobiphenyl-4-yl)-N-hydroxy-2-phenylacetamide | HCID 57779613 | 48% |
반응 단계
To a solution of 13 (40 mg, 0.14 mmol), BOP (58 mg, 0.13 mmol), and hydroxylamine hydrochloride (9 mg, 0.13 mmol) in pyridine (5 mL) was added triethylamine (0.055 mL, 0.39 mmol) and the reaction mixture was stirred at room temperature for 2 h. The solvents were removed under vacuum and the crude was dissolved in ethyl acetate. The organic layer was washed with water, dried over Na2SO4, filtered and concentrated. The residue was purified via HPLC (Gilson) reverse-phase column with a gradient of methanol (20-75%) in water to afford compound 14 as a white solid (20 mg, 48%). 1H NMR (CD3OD-d4) δ (ppm): 7.62-7.57 (m, 2H), 7.53 (d, J=8.2 Hz, 2H), 7.40-7.22 (m, 7H), 7.14 (t, J=8.8 Hz, 2H), 4.82 (s, 1H). LRMS (ESI): (calc.) 321.1 (found) 320.4 (MH)−.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09096565B2 |
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| 출처 데이터셋 | uspto-grants-2015_08 |
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| ORD ID | ord-9f596383458f40dab57e980dd79d8e61 |
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| 출처 메모 | uspto-grants-2015_08 |
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