関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | P-Cresol | HCID 2879 | — |
| 反応物 | Ethyl dichloroacetate | HCID 10808 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Ethyl 2,2-bis(4-methylphenoxy)acetate | HCID 23338923 | 77.3% |
反応手順
Sodium (5.7 g) is dissolved in ethanol (160 cc), and a solution of para-cresol (27 g) in ethanol (20 cc) is added. The mixture is stirred for 1 hour at 20° C. and ethyl dichloroacetate (20 g) in solution in ethanol (20 cc) is then added. The mixture is heated under reflux for 20 hours and then allowed to cool. The white precipitate obtained is filtered off and the filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C. The oil thus obtained is taken up in diethyl ether (300 cc) and washed twice with N sodium hydroxide solution (100 cc each time) and twice with distilled water (100 cc each time). The ethereal phase is then dried over anhydrous sodium sulphate, filtered, and concentrated to dryness under reduced pressure (20 mmHg) at 40° C. Ethyl 2,2-bis(4-methylphenoxy)acetate (29 g) is thus obtained as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04225589 |
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| 出典データセット | uspto-grants-1980_09 |
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| ORD ID | ord-b1d0998d3cf545b793e561524dc0c9a6 |
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| 出典メモ | uspto-grants-1980_09 |
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