関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethyl 2-oxocyclopentanecarboxylate | HCID 69136 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | Ethyl 1-methyl-2-oxocyclopentane-1-carboxylate | HCID 227353 | 99.4% |
反応手順
Under vigorously agitation, 20.3 g of ethyl 2-oxocyclopentane carboxylate was added to 53.8 g of fine powdery anhydrous potassium carbonate, and after stirring for several minutes, to the mixture was added 90 ml of acetone. The reaction mixture was further stirred for 15 to 30 minutes at room temperature, then to the mixture was dropwise added 36.9 g of methyl iodide. Upon the completion of the addition, the reaction mixture was heated for reflux for 1 hour. The solvent was removed under reduced pressure, and the solid residue was washed with diethyl ether. The washing liquor was collected and washed with water. After removing the solvent, 22.0 g of pale yellow liquid was obtained. The liquid was distilled under reduced pressure, and 20.9 g of colorless liquid as a distillate cut of 131-133° C./39 mmHg was collected. Yield: 94.6%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07388103B2 |
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| 出典データセット | uspto-grants-2008_06 |
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| ORD ID | ord-2e8967f0cb8b4592809b590ce6d184a7 |
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| 出典メモ | uspto-grants-2008_06 |
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