関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 反応物 | 4-Methylhept-2-enoic acid | HCID 21720203 | — |
| 反応物 | 2-Methoxy-4-piperazin-1-yl-quinoline | HCID 66835874 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (E)-1-[4-(2-Methoxy-4-quinolyl)piperazin-1-yl]-4-methyl-hept-2-en-1-one | HCID 56948961 | 40% |
反応手順
(E)-4-Methyl-hept-2-enoic acid (21.3 mg, 0.15 mmol) was dissolved in DMF (350 μl), diisopropylethylamine was added (26 μl, 0.15 mmol) followed by HATU (57 mg, 0.15 mmol dissolved in 0.25 ml DMF). The mixture was stirred at room temperature for 15 minutes, then 2-methoxy-4-piperazin-1-yl-quinoline (36.4 mg, 0.15 mmol, dissolved in 1 ml DMF) was added and stirring was continued overnight. The mixture was evaporated under reduced pressure, the residue was dissolved in dichloromethane and the resulting solution was washed with 5% sodium bicarbonate solution, water, evaporated to dryness under reduced pressure. The residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile) to yield 21.1 mg (0.06 mmol, 39.8%) of a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08883791B2 |
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| 出典データセット | uspto-grants-2014_11 |
|---|
| ORD ID | ord-32aec6e0d04d40cf81c859d5b8092f64 |
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| 出典メモ | uspto-grants-2014_11 |
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