関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dipropylamine | HCID 8902 | — |
| 反応物 | 2-Chloro-6-methylpyridine-4-carbonitrile | HCID 21085439 | — |
| 生成物 | 2-Chloro-6-methylpyridine-4-carbonitrile | HCID 21085439 | — |
| 生成物 | 2-(Dipropylamino)-6-methylisonicotinonitrile | HCID 21085459 | — |
反応手順
To 2-chloro-6-methylisonicotinonitrile (0.230 g, 1.51 mmol) was added di-n-propylamine (5 mL). The mixture was heated at 80° C. in a sealed, thick-walled glass vessel for 12 h and then at room temperature for 17 h. Excess di-n-propylamine was removed under reduced pressure and the residue was partitioned between dichloromethane and aq. sodium bicarbonate. After drying over sodium sulfate and concentration, the residue was chromatographed on silica gel using ethyl acetate-hexane (10/90) to give 0.14 g of 2-chloro-6-methylisonicotinonitrile and 0.059 g of 2-(dipropylamino)-6-methylisonicotinonitrile. Using the above conditions, 2-chloro-6-methylisonicotinonitrile (0.14 g) was converted to an additional 0.043 g of 2-(dipropylamino)-6-methylisonicotinonitrile.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07176242B2 |
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| 出典データセット | uspto-grants-2007_02 |
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| ORD ID | ord-3d9301bff211417b9038a604211b92d1 |
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| 出典メモ | uspto-grants-2007_02 |
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