関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl Ethyl Ketone | HCID 6569 | — |
| 反応物 | Diethyl Oxalate | HCID 7268 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 生成物 | Ethyl-2,4-dioxohexanoate | HCID 61590 | — |
反応手順
To a solution of sodium ethoxide (2.33 g, 34 mmol) in absolute alcohol (40 mL) was added a mixture of 2-butanone (2.45 g, 34 mmol) and diethyl oxalate (5 g, 34 mmol) dropwise at −5° C. The reaction mixture was stirred at −5° C. overnight and then concentrated. The resulting residue was partitioned between water (20 mL) and ethyl acetate (70 mL*3). The aqueous layer was acidified to pH 2 with dilute H2SO4 and then extracted with ethyl acetate (50 ml*3). The combined organic phase was dried over anhydrous Na2SO4, The organic solvent was evaporated in vacuo, and the residue was used directly in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09353104B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-fb116f77f42e4e2a81f6e943556c5890 |
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| 出典メモ | uspto-grants-2016_05 |
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