Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → N-[1-(4'-chloro-2'-fluoro-1,1'-biphenyl-2-yl)ethyl]-3-methoxybenzenesulfonamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 3-Methoxybenzenesulfonyl chloride | HCID 2737504 | — |
| 반응물 | 1-(4'-Chloro-2'-fluoro-biphenyl-2-yl)-ethylamine | HCID 22482361 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | N-[1-(4'-chloro-2'-fluoro-1,1'-biphenyl-2-yl)ethyl]-3-methoxybenzenesulfonamide | HCID 22482365 | 103.3% |
반응 단계
3-Methoxybenzenesulfonyl chloride (331 mg, 1.6 mmol) was added to a solution of 1-(4′-chloro-2′-fluoro-1,1′-biphenyl-2-yl)ethylamine (400 mg, 1.6 mmol) and triethylamine (246 μL, 1.7 mmol) in acetonitrile. The reaction was mixed at room temperature for 24 hours, afterwhich the acetonitrile was removed in vacuo. The remaining solid was dissolved in dichloromethane and purified by preparative liquid chromatogrpahy on a Biotage® 40 Mi column of prepacked silica gel (90 g), eluting with a gradient of 5%-50% methyl tert-butyl ether in hexane (35 min), to afford the the desired product (694 mg, 99%) as a white solid;
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06894061B2 |
| 출처 데이터셋 | uspto-grants-2005_05 |
| ORD ID | ord-b214738d486547c9bd54ab946152c525 |
| 출처 메모 | uspto-grants-2005_05 |