関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 反応物 | 4-Bromo-1-fluoro-2-nitrobenzene | HCID 2736328 | — |
| 反応物 | Potassium phthalimide | HCID 3356745 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(4-Bromo-2-nitrophenyl)isoindoline-1,3-dione | HCID 118025458 | 92% |
反応手順
4-bromo-1-fluoro-2-nitrobenzene (2.0 g, 9.1 mmol) and potassium 1,3-dioxoisoindolin-2-ide (2.0 g, 10.9 mmol) were placed in microwave vial (0.5-2 ml) and NMP (12.0 ml) was added. The reaction mixture was heated at 200° C. using microwave (Biotage, Initiator) for 1 min. After cooling to rt, the reaction mixture was added dropwise to stirring water which resulted in formation of precipitate. The solid was collected, washed with water and dried under stream of nitrogen to afford the title compound (2.89 g, yield: 92%). 1H-NMR (400 MHz, CDCl3) δ 7.26 (s, 2H) 7.43 (d, 2H) 7.81-7.87 (m, 3H) 7.91 (dd, 2H) 7.95-8.05 (m, 3H) 8.33 (d, 1H)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09434697B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
|---|
| ORD ID | ord-fdc4f6b5c93549c096c14e068b7f3621 |
|---|
| 出典メモ | uspto-grants-2016_09 |
|---|