化工社化工社 化学情報印刷レポート · 研究参考用
Iodine → N-(4-iodo-3-methylphenyl)-N-methylmethanesulphonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Iodic acid | HCID 24345 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | N-Methyl-N-(3-tolyl)methanesulphonamide | HCID 19785598 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-(4-iodo-3-methylphenyl)-N-methylmethanesulphonamide | HCID 19785617 | 340% |
反応手順
A solution of N-methyl-N-(3-tolyl)methanesulphonamide (0.12 g), iodine (76 g) and iodic acid (35 mg) in glacial acetic acid (5 ml) and concentrated sulphuric acid (0.6 ml) was stirred at 80° C. for 2.5 hours. Ethyl acetate (40 ml) and water (40 ml) were then added and the mixture neutralised with solid sodium bicarbonate. The organic phase was washed with brine (30 ml), dried (MgSO4) and the solvent evaporated to leave N-(4-iodo-3-methylphenyl)-N-methylmethanesulphonamide (0.22 g, 90%), m.p. 85°-87° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05258399 |
| 出典データセット | uspto-grants-1993_11 |
| ORD ID | ord-446eddc3b81e48e8876107b742a089a5 |
| 出典メモ | uspto-grants-1993_11 |