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1-Hydroxybenzotriazole → 4-Chloro-2-[(cyclopropylmethyl)aminocarbonyl]pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | (Cyclopropylmethyl)ammonium chloride | HCID 81671 | — |
| 反応物 | 4-Chloropyridine-2-carboxylic acid | HCID 230890 | — |
| 反応物 | 1-(3-Diethylaminopropyl)-3-ethylcarbodiimide hydrochloride | HCID 9964512 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 4-Chloro-2-[(cyclopropylmethyl)aminocarbonyl]pyridine | HCID 34829121 | — |
反応手順
4-Chloro-2-carboxypyridine (2.0 g), (aminomethyl)cyclopropane hydrochloride (1.7 g), 1-ethyl-3-(3-diethylaminopropyl)carbodiimide hydrochloride (WSC) (2.9 g), 1-hydroxybenzotriazole (HOBt) (2.3 g), triethylamine (2.1 ml) and tetrahydrofuran (30 ml) were stirred together at room temperature for 2 hours. Water was added, extraction was performed with ethyl acetate, and then silica gel was added to the extract and the solvent was distilled off under reduced pressure. The silica gel was charged into a dry column packed with silica gel and purified by column chromatography (hexane:ethyl acetate=4:1, followed by 2:1) to obtain 1.5 mg of the target substance as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08372981B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-b268e0e64c834e73af0da496495d3866 |
| 出典メモ | uspto-grants-2013_02 |