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Methylamine → 4-fluoro-N-methylbenzene-1-sulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Fluorobenzenesulfonyl chloride | HCID 9588 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-fluoro-N-methylbenzene-1-sulfonamide | HCID 2440054 | 95.1% |
反応手順
A mixture of 125 ml of methylamine (0.25 molar) in tetrahydrofuran and 13.9 ml (0.10 mol) of triethylamine was chilled in an ice bath. To this chilled solution was added dropwise 19.4 g (0.10 mol) of 4-fluorobenzenesulfonyl chloride in 150 ml of CH2Cl2 was added and the mixture refluxed for 2 hours and then stirred overnight at room temperature. The mixture was with CH2Cl2, washed with H2O, 2N citric acid, brine and dried (Na2SO4). The solution was filtered through a pad of hydrous magnesium silicate and the filtrate concentrated to dryness under vacuum to give 18.0 g of white solid, mp 67-70° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06946473B2 |
| 出典データセット | uspto-grants-2005_09 |
| ORD ID | ord-76b8047aab694b01b80a5d6ed2ffd4d9 |
| 出典メモ | uspto-grants-2005_09 |