Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pyridine → 2-amino-5-bromo-N,N-dimethylpyridine-3-sulfonamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Benzenesulfonyl chloride | HCID 7369 | — |
| 반응물 | 2-Aminopyridine | HCID 10439 | — |
| 반응물 | 3-Amino-5-bromo-2-chloropyridine | HCID 21858354 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-amino-5-bromo-N,N-dimethylpyridine-3-sulfonamide | HCID 52335153 | 34% |
반응 단계
To a stirred solution of a pyridineamine such as 3-amino-5-bromo-2-chloropyridine (24 mmol) in dichloromethane (50 mL) was added pyridine (37 mmol) followed by benzenesulfonyl chloride (35 mmol) dropwise over 5 minutes. The reaction mixture was stirred at RT for 18 h and evaporated to dryness in vacuo. The residue was purified by flash chromatography on silica gel (15% hexanes in CH2Cl2 then 0 to 5% EtOAc in 15% hexanes in CH2Cl2). During evaporation of the solvents the product crashed out. The resultant slurry was diluted with hexanes, filtered and dried under vacuum to give the title compound (2.89 g, 34%) as a white solid. MS (ES) m/e 346.7 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07592342B2 |
| 출처 데이터셋 | uspto-grants-2009_09 |
| ORD ID | ord-3afc9affb6774934b835188b36274753 |
| 출처 메모 | uspto-grants-2009_09 |