関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | N-[1-(2',4'-Difluoro-1,1'-biphenyl-2-yl)ethyl]4-methoxybenzenesulfonamide | HCID 22482282 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Fluoro-5-[(4-methoxyphenyl)sulfonyl]-6-methyl-5,6-dihydrophenanthridine | HCID 22482323 | 98.3% |
反応手順
N-[1-(2′,4′-Difluoro-1,1′-biphenyl-2-yl)ethyl]4-methoxybenzenesulfonamide (347 mg, 0.86 mmol) was dissolved in anhydrous N,N-dimethylformamide (2 mL) and potassium carbonate (238 mg, 1.72 mmol) was added as a solid in one portion. The mixture was heated at 100° C. with stirring until a single product had formed as gauged by LCMS (5-6 hours). Water (10 mL) was added and a white solid precipitated from the cloudy solution. The mixture was allowed to stand until the solution was clear, and the precipitated solid was filtered and washed with additional water to afford the desired compound (324 mg, 98%) as a white solid, m.p. 137.5-139° C.;
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06894061B2 |
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| 出典データセット | uspto-grants-2005_05 |
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| ORD ID | ord-8f7a79e8c94445db8000f2092601fa74 |
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| 出典メモ | uspto-grants-2005_05 |
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