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Iodine → 4-Methoxy-3-hydroxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone
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-Methoxy-3-hydroxy-2-(1-methyl-1-phenylethyl)isoindolinone | HCID 68488636 | — |
| 反応物 | HCID 178444656 | HCID 178444656 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Methoxy-3-hydroxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone | HCID 68491173 | 77% |
反応手順
In a similar manner to Step 3 of Example 16, 4-methoxy-3-hydroxy-2-(1-methyl-1-phenylethyl)isoindolinone (3.55 g, 11.9 mmol) was dissolved in THF (140 mL), and the solution was treated with TMEDA (4.00 mL, 26.2 mmol), sec-butyllithium-hexane solution (0.99 mol/L, 26.4 mL, 26.2 mmol) and iodine (3.62 g, 14.3 mmol), followed by purification by flash column chromatography (hexane/ethyl acetate=9/1, 7/3) to obtain 4-methoxy-3-hydroxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone (3.88 g, yield 77%).
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-81f75ec20d134ed9b2b858fa950481b5 |
| 出典メモ | uspto-grants-2010_06 |