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Water → 7-Amino-4-bromo-3-hydroxyisoindolinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Diisobutylaluminumhydride | HCID 21225700 | — |
| 反応物 | 4-amino-7-bromo-2,3-dihydro-1H-isoindole-1,3-dione | HCID 68489089 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 7-Amino-4-bromo-3-hydroxyisoindolinone | HCID 68491045 | 72.1% |
反応手順
3-Amino-6-bromophthalimide (3.10 g, 12.9 mmol) was dissolved in THF (240 mL), and the solution was added with diisobutylaluminiumhydride (0.94 mol/L, 68.6 mL, 64.5 mmol) by drops at −78° C. for 25 minutes, then the reaction mixture was warmed to room temperature, followed by stirring for 1.5 hours. Then, the reaction mixture was ice-cooled, added with water and filtered using Celite. The filtrate was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by slurry using chloroform to obtain 7-amino-4-bromo-3-hydroxyisoindolinone (2.26 g, yield 72%).
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-07fff94954834be4b0ddba67b532291f |
| 出典メモ | uspto-grants-2010_06 |