関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1-(6-Chloropyridin-3-yl)ethan-1-one | HCID 2779698 | — |
| 反応物 | (S)-3-(2,5-difluoro-4-(methylsulfonyl)phenylamino)-1,4'-bipiperidin-2-one hydrochloride | HCID 66803298 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 67470532 | HCID 67470532 | 68.6% |
反応手順
(S)-3-(2,5-difluoro-4-(methylsulfonyl)phenylamino)-1,4′-bipiperidin-2-one hydrochloride (Example 45, Steps A-E; 0.4 g, 0.944 mmol), 1-(6-chloropyridin-3-yl)ethanone (0.220 g, 1.42 mmol) and DIEA (0.523 mL, 2.83 mmol) were dissolved in DMF (5 mL) and heated at 100° C. overnight. The reaction was concentrated and purified over silica gel (50-100% EtOAc in hexanes) to afford (S)-1′-(5-acetylpyridin-2-yl)-3-(2,5-difluoro-4-(methylsulfonyl)phenylamino)-1,4′-bipiperidin-2-one (0.328 g, 0.647 mmol, 68.6% yield) as yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08754226B2 |
|---|
| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-dffa7671968941d08b307477900251d0 |
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| 出典メモ | uspto-grants-2014_06 |
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