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Diisopropylethylamine → 4-(5'-Bromo-3'-fluoro-2,3,5,6-tetrahydro-[1,2']bipyridinyl-4-ylideneaminooxy)-piperidine-1-carboxylic acid isopropyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 5-Bromo-2-chloro-3-fluoropyridine | HCID 2763285 | — |
| 反応物 | Isopropyl 4-(Piperidin-4-ylideneaminooxy)piperidine-1-carboxylate | HCID 57461147 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 4-(5'-Bromo-3'-fluoro-2,3,5,6-tetrahydro-[1,2']bipyridinyl-4-ylideneaminooxy)-piperidine-1-carboxylic acid isopropyl ester | HCID 86655009 | 28.3% |
反応手順
2d (0.22 g, 0.71 mmol), 3-bromo-6-chloro-5-fluoro-pyridine (0.2 g, 0.95 mmol) and diisopropylethylamine (0.2 mL, 1.2 mmol) in 2 mL of DMSO were heated at 130° C. for 20 h. The mixture was cooled to room temperature and purified by flash LC(0 to 30% EtOAc+0.1% triethylamine in hexane) to afford 46a (92 mg, 28% yield): HPLC, LC-MS 457.1 (MH).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08293729B2 |
| 出典データセット | uspto-grants-2012_10 |
| ORD ID | ord-65461793d462409bbd3185334507dcd5 |
| 出典メモ | uspto-grants-2012_10 |