関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Sulfide | HCID 14804 | — |
| 反応物 | 4-(3-Fluoropyridin-4-yl)benzonitrile | HCID 10856435 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(3-Mercaptopyridin-4-yl)benzonitrile | HCID 67997061 | 96% |
反応手順
A mixture of 4-(3-fluoropyridin-4-yl)benzonitrile (1.08 g, 5.4 mmol) and sodium sulfide (0.84 g, 10.8 mmol) in DMF (20 mL) was stirred at 130° C. for 0.5 hours. While the reaction was cooled in ice water bath, aqueous HCl (6N, 2.5 mL) was added drop wise with rigorous stirring. The resulting yellow paste was concentrated using rotary evaporation on a water bath (80° C.) to dryness. The resulting yellow solid was extracted with methanol (4×20 mL). The combined extracts were concentrated to dryness to give a yellow solid (1.1 g, 96%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08541589B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-dfe61e8317574b2dbb0f1e3faa3d24a2 |
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| 出典メモ | uspto-grants-2013_09 |
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