関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Pentanol | HCID 6276 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2'-Bromoacetophenone | HCID 75060 | — |
| 反応物 | 2,3-Dimethoxyphenol | HCID 78828 | — |
| 触媒 | Cupric acetate | HCID 8895 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-(2,3-Dimethoxyphenoxy)acetophenone | HCID 18379955 | 87% |
反応手順
Amyl alcohol (44 ml) was added to 2,3-dimethoxyphenol (5 g), 2'-bromoacetophenone (7 g), potassium carbonate (6.7 g) and copper acetate (1.1 g), followed by heating and stirring at 150° C. for 8 hours for reacting them together. To the reaction solution was added ethyl acetate (300 ml), and the resulting solution was washed in dilute hydrochloric acid, in water, and in a saturated sodium chloride solution, and dried over anhydrous magnesium sulfate, and the solvents therein were distilled off under reduced pressure. The residue was purified by silica gel column chromatography (developing solvent: hexane:ethyl acetate=8:1), to recover 2-(2,3-dimethoxyphenoxy)acetophenone (7.6 g; yield of 87%). By 1H-NMR (90 MHz, CDCl3), the compound has the peaks shown below.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05734067 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-b4abd6c40e154847ac62183456b57efd |
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| 出典メモ | uspto-grants-1998_03 |
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