Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Hydroxybenzotriazole → 4-Chloro-2-[(cyclopropylmethyl)aminocarbonyl]pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | (Cyclopropylmethyl)ammonium chloride | HCID 81671 | — |
| 반응물 | 4-Chloropyridine-2-carboxylic acid | HCID 230890 | — |
| 반응물 | 1-(3-Diethylaminopropyl)-3-ethylcarbodiimide hydrochloride | HCID 9964512 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | 4-Chloro-2-[(cyclopropylmethyl)aminocarbonyl]pyridine | HCID 34829121 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07612092B2 |
| 출처 데이터셋 | uspto-grants-2009_11 |
| ORD ID | ord-d4be9d575dae478c84c8674a87194404 |
| 출처 메모 | uspto-grants-2009_11 |