関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Diethyl Carbonate | HCID 7766 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-(3-(Phenylmethoxy)phenyl)ethan-1-one | HCID 98689 | — |
| 生成物 | Ethyl 3-[3-(benzyloxy)phenyl]-3-oxopropanoate | HCID 10334847 | 84% |
反応手順
1-(3-Benzyloxyphenyl)ethanone (218 g, 966.10 mmol) was dissolved in diethyl carbonate and sodium hydride (60% oil) (46.37 g, 1.15 mmol) was slowly added thereto at 0° C., and then stirred for 3 hours at 60° C. After the reaction was completed, ice water and acetic acid were added to the reaction mixture, extracted with ethyl acetate/saturated sodium chloride, the organic layer was separated, and dried over anhydrous magnesium sulfate. The solvent was removed under a reduced pressure and the resulting residue was purified by column chromatography (ethyl acetate:hexane=1:10) to obtain 3-(3-benzyloxyphenyl)-3-oxopropionate ethyl ester (184.68 g, yield 84%) in an oil state.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07741323B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-444829afa1d64032803c8a8149fb905d |
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| 出典メモ | uspto-grants-2010_06 |
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