関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3-Pyridinecarboxaldehyde | HCID 10371 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Butanone, 1-(4-chlorophenoxy)-3,3-dimethyl- | HCID 90518 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-(4-Chlorophenoxy)-4,4-dimethyl-1-pyridin-3-yl-1-penten-3-one | HCID 54241059 | 72.2% |
反応手順
100 ml of water, followed by 28 ml of 10% strength aqueous sodium hydroxide solution, were added to a stirred solution of 22.6 g (0.1 mol) of 1-(4-chlorophenoxy)-3,3-dimethyl-butan-2-one and 21.4 g (0.2 mol) of 3-pyridinealdehyde in 500 ml of methanol. The solution was subsequently stirred at room temperature for 4 days, the methanol was removed in vacuo and the aqueous residue was taken up in ether. The aqueous phase was separated off, the organic phase was extracted three times with 1 N hydrochloric acid and the hydrochloric acid extracts were neutralized with solid sodium bicarbonate and extracted three times with ethyl acetate. 22.8 g (72% of theory) Of 2-(4-chlorophenoxy)-4,4-dimethyl-1-pyridin-3-yl-1-penten-3-one of melting point 74°-76° C. were obtained from the ethyl acetate phase.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04262000 |
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| 出典データセット | uspto-grants-1981_04 |
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| ORD ID | ord-57ed26b9f8c64311ad3785c3d0600b05 |
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| 出典メモ | uspto-grants-1981_04 |
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