関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Ethylcyclohexyl(oxo)acetate | HCID 11041407 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | alpha-Oxocyclohexaneacetic acid | HCID 78060 | 100% |
反応手順
To a solution of ethyl cyclohexyloxoacetate (46 g) in MeOH (25 mL) was added water (60 mL) and NaOH (50% 20 mL) at 0-15° C. The reaction mixture was heated to 60° C. for 1.5 h. The reaction mixture was cooled with ice-water bath, and acidified with 15% HCl till pH 1. The mixture was extracted with ethyl acetate (2×250 mL). The extracts were washed with brine, dried with sodium sulfate. The drying agent was removed by filtration and the solvent was removed to give a low melting solid (39 g, 99%). 1H NMR: δ 1.15-1.40 (m, 5H,), 1.62-1.96 (m, 5H). 3.20 (m, 1H), 9.4 (s, 1H). 13C-NMR δ, 25.93, 25.76, 27.89, 45.04, 160.90, 198.29.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06025177 |
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| 出典データセット | uspto-grants-2000_02 |
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| ORD ID | ord-dcd8cbebc73e414fa1400d84c56ff23c |
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| 出典メモ | uspto-grants-2000_02 |
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