関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Trifluoroacetic anhydride | HCID 9845 | — |
| 反応物 | 2-Amino-6-chloropyridine-3-carbaldehyde oxime hydrochloride | HCID 86635021 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | 2-Amino-6-chloropyridine-3-carbonitrile | HCID 20311686 | — |
反応手順
11.15 g (53.6 mmol) of 2-amino-6-chloropyridine-3-carbaldehyde oxime hydrochloride (Example 27A) were initially charged in dioxane, 13 ml (161 mmol) of pyridine were added and the mixture was cooled to 0° C. 8.3 ml (58.95 mmol) of trifluoroacetic anhydride were added, and the reaction was warmed to RT and then stirred at 60° C. for 2 h. The reaction mixture was taken up in a mixture of ethyl acetate and sodium bicarbonate solution. The organic phase was washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate and concentrated on a rotary evaporator. The residue was suspended in dichloromethane:diethyl ether 3:1, and the solid was filtered off with suction and dried. This gave 5.56 g (66% of theory) of the product as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08476267B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-b64671c2b5694f00acfa2cdc97cdcd23 |
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| 出典メモ | uspto-grants-2013_07 |
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