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Triethylamine → N-[1-(4'-chloro-2'-fluoro-1,1'-biphenyl-2-yl)ethyl]-3-methoxybenzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Methoxybenzenesulfonyl chloride | HCID 2737504 | — |
| 反応物 | 1-(4'-Chloro-2'-fluoro-biphenyl-2-yl)-ethylamine | HCID 22482361 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | N-[1-(4'-chloro-2'-fluoro-1,1'-biphenyl-2-yl)ethyl]-3-methoxybenzenesulfonamide | HCID 22482365 | 103.3% |
反応手順
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;
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06894061B2 |
| 出典データセット | uspto-grants-2005_05 |
| ORD ID | ord-b214738d486547c9bd54ab946152c525 |
| 出典メモ | uspto-grants-2005_05 |