関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | N-hydroxybenzenecarboximidoyl chloride | HCID 2756315 | — |
| 反応物 | 1-(2-Bromopyridin-4-yl)propan-2-one | HCID 23435643 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-Bromo-4-(5-methyl-3-phenyl-isoxazol-4-yl)-pyridine | HCID 23435665 | 52.4% |
反応手順
To a stirred solution of Compound 16 (1.71 g, 8.0 mmol) and Et3N (2.23 mL, 16 mmol) in EtOH (16 mL) was added a solution of benzoylchloride oxime (1.62 g, 10.4 mmol) in EtOH (16 mL) over 90 min. The solution was stirred at 25° C. for 90 min. Then, the solution was heated to reflux for 24 h. The solution was cooled to 25° C. and concentrated. The crude material was taken up in CH2Cl2 (50 mL) and poured into saturated aqueous NaHCO3 (50 mL), extracted with CH2Cl2 (3×50 mL), dried (Na2SO4), and filtered. Flash chromatography (SiO2, 20% EtOAc-hexanes) provided the title compound (1.32 g, 4.19 mmol, 52%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07169798B2 |
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| 出典データセット | uspto-grants-2007_01 |
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| ORD ID | ord-9300128f3e0144c191cb7471cf6d67b0 |
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| 出典メモ | uspto-grants-2007_01 |
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