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Potassium Iodide → 1-(2-Hydroxy-4-((4-methoxyphenyl)methoxy)phenyl)ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | 2',4'-Dihydroxyacetophenone | HCID 6990 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Methyloxybenzyl chloride | HCID 69993 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(2-Hydroxy-4-((4-methoxyphenyl)methoxy)phenyl)ethanone | HCID 11323232 | — |
反応手順
2′,4′-Dihydroxyacetophenone (11.71 g, 0.077 mol), 4-methoxybenzyl chloride (10.44 ml, 0.077 mol), anhydrous potassium carbonate (11.75 g, 0.085 mol) and potassium iodide (12.78 g, 0.077 mol) are heated together in refluxing dry acetone (80 ml) for 4 hours. The mixture is then cooled to room temperature, poured into water (250 ml) and extracted with ethyl acetate (3×100 ml). The ethyl acetate extracts are combined, washed with saturated brine (100 ml), dried (MgSO4), filtered and concentrated, until crystallization commences. After standing at 4° C. for 16 h, the crystals are recovered by filtration, washed with cold ethyl acetate and then with n-hexane and dried.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07732435B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-7b4b11184e3f449b88142c800caa6db1 |
| 出典メモ | uspto-grants-2010_06 |