関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine-2-carbonitrile | HCID 7522 | — |
| 反応物 | 4-(Methylsulfonyl)aniline hydrochloride | HCID 2735180 | — |
| 反応物 | Trimethylaluminum | HCID 16682925 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | HCID 178504797 | HCID 178504797 | — |
反応手順
To a suspension of 4-(methylsulfonyl)aniline hydrochloride (6 g, 28.8 mmol) in toluene (150 ml) at 0° C., trimethylaluminum (2M solution in toluene, 21.6 ml, 43.2 mmol) was added over 15 minutes. The reaction mixture was warmed to room temperature and stirred for 2.5 hours. A solution of 2-cyanopyridine (6 g, 57.6 mmol) in toluene (150 ml) was added over 10 minutes and the reaction mixture was heated to 85°-90° C. After 24 hours, the reaction mixture was cooled to room temperature and poured over a slurry of silica gel in chloroform. After filtration, the residue was washed with a mixture of methylene chloride/methanol and later methanol. The combined filtrates were concentrated and the resulting yellowish solid was stirred with ethyl acetate (1500 ml) and filtered. The pale yellow solid (5.2 g, 66%) was used in the next reaction without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05616601 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-5222de9267fa43ebad89cdeb17a5147f |
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| 出典メモ | uspto-grants-1997_04 |
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