関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-(3-Chlorophenyl)ethanone | HCID 14933 | — |
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 反応物 | 1-(4-Chlorophenyl)-3,3-bis(methylsulfanyl)prop-2-en-1-one | HCID 2807379 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Pyridine, 2-(3-chlorophenyl)-6-(4-chlorophenyl)-4-(methylthio)- | HCID 189415 | 74.7% |
反応手順
To 20 ml of tetrahydrofuran solution containing 0.60 g of m-chloroacetophenone was added 1.0 g of potassium t-butoxide at room temperature, followed by stirring for 30 minutes. Further, 1 g of 3,3-bis-(methylthio)-1-(4'-chlorophenyl)-2-propen-1-one was added, followed by stirring for 1 hour. Subsequently, 20 ml of acetic acid and 3 g of ammonium acetate were added, and reaction was carried out for 3 hours under reflux, while distilling away tetrahydrofuran. The reaction liquid was neutralized with an aqueous solution of sodium hydroxide, and the neutralized solution was extracted twice with 50 ml portions of ethyl acetate. The extract was dried with anhydrous magnesium sulfate. Ethyl acetate was distilled away under reduced pressure and the residues were recrystallized from isopropanol to give 1.0 g of 2-(3'-chlorophenyl)-4-methylthio-6-(4'-chlorophenyl)pyridine. (m.p. 98.4° C.)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04849011 |
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| 出典データセット | uspto-grants-1989_07 |
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| ORD ID | ord-909260d93b1f4efa888fa7ce6d7ca364 |
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| 出典メモ | uspto-grants-1989_07 |
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