化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → N-(4-chloro-3-nitrophenyl)methanesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Chloro-3-nitroaniline | HCID 12477 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | N-(4-chloro-3-nitrophenyl)methanesulfonamide | HCID 3755760 | 78.1% |
反応手順
Methanesulphonyl chloride (58.3 g, 0.509 mole) was added in one portion to a stirred solution of 97% 4-chloro-3-nitroaniline (86 g, 0.485 mole) in pyridine (80 ml) and xylene (500 ml). The temperature rose to 50° and the mixture was allowed to stand for a further 2 hr before addition of a mixture of 10M-hydrochloric acid (100 ml) and water (100 ml). The brown solid which was collected and washed successively with xylene (50 ml) and water (3×50 ml). The damp material was crystallized from methanol (800 ml) to give a solid which was collected, washed with methanol (2×50 ml) and dried to give the product 95 g (78%) m.p. 163°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05021333 |
| 出典データセット | uspto-grants-1991_06 |
| ORD ID | ord-72e351e850fe4f548665b422a5a79849 |
| 出典メモ | uspto-grants-1991_06 |