참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 1-(3-Chlorophenyl)ethanone | HCID 14933 | — |
| 반응물 | Ammonium Acetate | HCID 517165 | — |
| 반응물 | 1-(4-Chlorophenyl)-3,3-bis(methylsulfanyl)prop-2-en-1-one | HCID 2807379 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Pyridine, 2-(3-chlorophenyl)-6-(4-chlorophenyl)-4-(methylthio)- | HCID 189415 | 74.7% |
반응 단계
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.)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04849011 |
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| 출처 데이터셋 | uspto-grants-1989_07 |
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| ORD ID | ord-909260d93b1f4efa888fa7ce6d7ca364 |
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| 출처 메모 | uspto-grants-1989_07 |
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