Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2-Amino-5-bromopyridine → N-(5-Bromopyridin-2-yl)-4-methanesulfonylbenzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2-Amino-5-bromopyridine | HCID 70622 | — |
| 반응물 | p-(Methylsulphonyl)benzoic acid | HCID 77670 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | N-(5-Bromopyridin-2-yl)-4-methanesulfonylbenzamide | HCID 60650971 | 32% |
반응 단계
To a solution of 4-methanesulfonylbenzoic acid (100 mg, 0.50 mmol) and 2-amino-5-bromopyridine (104 mg, 0.60 mmol) in dry dichloromethane (10 mL) was added 4-(dimethylamino)pyridine (67 mg, 0.55 mmol) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (105 mg, 0.55 mmol). The mixture was stirred at room temperature overnight under N2, diluted with water (10 mL) and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform/ethyl acetate=3/1) to give the title compound as a white crystal (56 mg, yield 32%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08536176B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-4c00404d38ee45448ee89b81e24fc793 |
| 출처 메모 | uspto-grants-2013_09 |