化工社化工社 化学情報印刷レポート · 研究参考用
Methanol → 4-iodo-1H-Isoindole-1,3(2H)-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Hexamethyldisilazane | HCID 13838 | — |
| 反応物 | 3-Iodophthalic anhydride | HCID 282071 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-iodo-1H-Isoindole-1,3(2H)-dione | HCID 18407512 | 68% |
反応手順
3-Iodophthalic anhydride (598 mg, 2.18 mmol) was dissolved in DMF (14 mL), and the solution was added with an aqueous solution (10 mL) of hexamethyldisilazane (HMDS) (4.6 mL, 22 mmol) and methanol (0.44 mL, 11 mmol), followed by stirring at room temperature for 18.5 hours. The reaction mixture was added with water and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure a and the residue was purified by slurry using chloroform to obtain 3-iodophtalimide (403 mg, yield 68%).
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-0ee272fea7cd425ebdbaa6a1eccbe4c9 |
| 出典メモ | uspto-grants-2010_06 |