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Methyl iodide → 2-Hydroxy-4-methoxybenzophenone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | 2,4-Dihydroxybenzophenone | HCID 8572 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Hydroxy-4-methoxybenzophenone | HCID 4632 | — |
反応手順
The above prepared (2,4-dihydroxy-phenyl)-phenyl-methanone (0.775 g, 3.62 mmol) was dissolved in 15 mL of acetonitrile and treated successively at 0° C. with Cs2CO3 (1.297 g, 1.1 eq.) and iodomethane (0.242 mL, 1.08 eq.), and the mixture was then stirred over night at ambient temperature. Pouring onto crashed ice/NH4Cl, twofold extraction with AcOEt, washing with water, drying over sodium sulfate, and evaporation of the solvents, followed by flash chromatography (SiO2, heptane/AcOEt=9/1), delivered 0.681 g of the title compound as off-white oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07534788B2 |
| 出典データセット | uspto-grants-2009_05 |
| ORD ID | ord-c7f63306a63f49d0aaaa50c748b9e9e7 |
| 出典メモ | uspto-grants-2009_05 |