関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl mercaptan | HCID 7509 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Chloronicotinonitrile | HCID 81079 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Pyridinecarbonitrile, 2-[(phenylmethyl)thio]- | HCID 501238 | — |
反応手順
85 g of 2-chloro-3-cyanopyridine, 98.2 g potassium carbonate anhydrous powder and 600 g of dimethyl formamide were mixed to obtain a suspension. To this suspension, a solution of 79.2 g benzyl mercaptan in 250 ml dimethyl formamide was added dropwise over a period of approx. 3 hours at 80-90° C. The reaction mass was agitated for 2 hours at the same temperature. The temperature was slowly raised to 120° C. Then, the reaction mixture was reacted at 120-130° C. for about 1.5 hours. Afterwards, heating was stopped and reaction mass was allowed to attain the room temperature. Inorganic cake was separated by filtration. Dimethyl formamide was distilled under reduced pressure, and the residue left at bottom was 2-(phenyl methyl thio)-3-cyano pyridine 150 g, sufficiently pure to be used in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07745631B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-cbcd9c92fadd44968fde6c4bac74bf3e |
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| 出典メモ | uspto-grants-2010_06 |
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