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Methyl iodide → 4-Iodo-2-methoxybenzyl alcohol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2-(Hydroxymethyl)-5-iodophenol | HCID 18779734 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Iodo-2-methoxybenzyl alcohol | HCID 18779792 | — |
反応手順
2-Hydroxy-4-iodo-benzylalcohol from Step 3 (1.0 g, 4.0 mmol), Cs2CO3 (1.3 g, 4.0 mmol) and iodomethane (0.25 mL, 4.0 mmol) were dissolved in DMF and heated to 800 for 1 hour and then stirred at room temperature for 2 hours. The DMF was removed in vacuo and the residue was partitioned between H2O and EtOAc. The aqueous layer was extracted with EtOAc (2×). The organic layers were combined, washed with H2O and brine, dried (MgSO4), filtered and concentrated to yield an oil. This oil was purified by flash chromatography eluting product with 30% EtOAC/Hexane to give the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05939439 |
| 出典データセット | uspto-grants-1999_08 |
| ORD ID | ord-ce4bbcbf7fd1473b8e7a14eb21f24383 |
| 出典メモ | uspto-grants-1999_08 |