関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 4,4'-Dichlorobenzhydrol | HCID 7033 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | HCID 178516071 | HCID 178516071 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-[Bis-(4-Chlorophenyl)-Methyl]-2-Pyridone | HCID 22748768 | — |
反応手順
Combine 50.6 g. (0.2 mole) of 4,4'-dichlorobenzhydrol with 57.1 g. (0.6 mole) of 2-hydroxy pyridine, with stirring heat to 200° C. and add dropwise 1.0 ml. of concentrated sulfuric acid. Increase the reaction temperature to 240°-250° C. and maintain at that temperature range while collecting water emanating from the reaction. Cool the reaction mixture, add a mixture of ethyl acetate and water with stirring and separate the liquid phases. Dry the organic phase, reduce the volume of ethyl acetate, cool to precipitate the crude product, yield 43 g. Crystallization from ethanol affords the product of this step, m.p. 211°-215° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04138488 |
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| 出典データセット | uspto-grants-1979_02 |
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| ORD ID | ord-b4ec73929dc04ea69628776727c52530 |
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| 出典メモ | uspto-grants-1979_02 |
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