化工社化工社 化学情報印刷レポート · 研究参考用
Diisopropylethylamine → 2-(((2S,3R)-3-Methyl-1-(5-methyl-2-(1-methyl-1H-pyrazol-4-yl)benzoyl)piperidin-2-yl)methyl)isoindoline-1,3-dione
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 | 5-Methyl-2-(1-methyl-1H-pyrazol-4-yl)benzoic acid | HCID 81111500 | — |
| 反応物 | 2-(((2S,3R)-3-Methylpiperidin-2-yl)methyl)isoindoline-1,3-dione | HCID 117727630 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(((2S,3R)-3-Methyl-1-(5-methyl-2-(1-methyl-1H-pyrazol-4-yl)benzoyl)piperidin-2-yl)methyl)isoindoline-1,3-dione | HCID 117727726 | — |
反応手順
A mixture of 2-(((2S,3R)-3-methylpiperidin-2-yl)methyl)isoindoline-1,3-dione (0.66 g, 2.55 mmol), 5-methyl-2-(1-methyl-1H-pyrazol-4-yl)benzoic acid (0.5 g, 2.318 mmol), diisopropylethylamine (0.7 mL, 6.954 mmol) and HATU (0.881 g, 2.318 mmol) in DCM was stirred at rt for 1 h. The reaction mixture was diluted with DCM and washed with satd. NaHCO3 and brine successively. The organic layer was separated, dried with MgSO4 and concentrated in vacuo. The crude product was purified by chromatography on silica gel (EtOAc/hexanes) to afford the title compound. ESI-MS (m/z): 457 [M+1]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09440982B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-ede6921068a743bc993a95aba548a219 |
| 出典メモ | uspto-grants-2016_09 |