化工社化工社 化学情報印刷レポート · 研究参考用
Iodine → HCID 68491790、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | N,N,N',N'-Tetramethylethylenediamine | HCID 8037 | — |
| 反応物 | 4-Fluoro-3-hydroxy-2-(1-methyl-1-phenylethyl)isoindolinone | HCID 68493841 | — |
| 反応物 | HCID 178444656 | HCID 178444656 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 68491790 | HCID 68491790 | 40% |
| 生成物 | 1-(1-Methyl-1-phenylethyl)-3-fluoro-6-iodophtalimide | HCID 131728234 | 14% |
反応手順
In a similar manner to Step 3 of Example 16, 4-fluoro-3-hydroxy-2-(1-methyl-1-phenylethyl)isoindolinone (2.06 g, 7.22 mmol) was dissolved in THF (80 mL), and the solution was treated with TMEDA (2.40 mL, 15.9 mmol), sec-butyllithium-hexane solution (0.99 mol/L, 16.0 mL, 15.9 mmol) and iodine (2.20 g, 8.66 mmol), followed by purification by flash column chromatography (chloroform/methanol=100/0, 85/15) to obtain 4-fluoro-3-hydroxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone (1.19 g, yield 40%) and 1-(1-methyl-1-phenylethyl)-3-fluoro-6-iodophtalimide (425 mg, yield 14%).
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-08104d4147f74fd5967f2101c4f10757 |
| 出典メモ | uspto-grants-2010_06 |