化工社化工社 化学情報印刷レポート · 研究参考用
Water → 7-Amino-4-bromo-2,3-dihydroisoindol-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | Triethylsilane | HCID 12052 | — |
| 反応物 | 7-Amino-4-bromo-3-hydroxyisoindolinone | HCID 68491045 | — |
| 溶媒 | Nitromethane | HCID 6375 | — |
| 生成物 | 7-Amino-4-bromo-2,3-dihydroisoindol-1-one | HCID 19701932 | 74.3% |
反応手順
7-Amino-4-bromo-3-hydroxyisoindolinone (3.11 g, 12.8 mmol) was dissolved in nitromethane (125 mL), and the solution was added with trifluoroacetic acid (9.90 mL, 128 mmol) and triethylsilane (4.10 mL, 25.6 mmol), followed by stirring at room temperature for 2 hours. The reaction mixture was added with water, extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium hydrogencarbonate solution and saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by slurry using chloroform to obtain 7-amino-4-bromoisoindolinone (2.16 g, yield 74%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07745641B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-dcddd7e42c624d299abe44804df57b43 |
| 出典メモ | uspto-grants-2010_06 |