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Potassium Fluoride → N-(5-((5-bromo-3-nitropyridin-2-yl)amino)-2',6'-difluoro-[1,1'-biphenyl]-3-yl)acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 反応物 | 5-Bromo-2-chloro-3-nitropyridine | HCID 7019412 | — |
| 反応物 | N-(5-amino-2',6'-difluoro-[1,1'-biphenyl]-3-yl)acetamide | HCID 89500157 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-(5-((5-bromo-3-nitropyridin-2-yl)amino)-2',6'-difluoro-[1,1'-biphenyl]-3-yl)acetamide | HCID 117777719 | 28% |
反応手順
A solution of N-(5-amino-2′,6′-difluoro-[1,1′-biphenyl]-3-yl)acetamide (1.4 g, 6.1 mmol), 5-bromo-2-chloro-3-nitropyridine (1.6 g, 6.1 mmol, 1.0 eq.) and potassium fluoride (0.53 g, 9.0 mmol, 1.5 eq.) in DMF (8 ml) was heated at 110° C. for 4 h. The mixture was quenched and extracted as in Example 1(d). The solvent was distilled off to afford the crude product which was purified by column chromatography (60-120 silica gel, 30% Ethyl acetate in hexane) to give the title product in 28% yield (0.8 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09447091B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-617f241a9e4c4fe1aee17f66a38e319f |
| 出典メモ | uspto-grants-2016_09 |