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Hydrochloric Acid → 3-(Dodecane-1-sulfonylamino)-4-methoxy-N-(3,4-dichloro-phenyl)-benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Dodecylsulfonyl chloride | HCID 66280 | — |
| 反応物 | 3-Amino-4-methoxy-N-(3,4-dichlorophenyl)-benzamide | HCID 9948627 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(Dodecane-1-sulfonylamino)-4-methoxy-N-(3,4-dichloro-phenyl)-benzamide | HCID 18626314 | 79.7% |
反応手順
Pyridine (5 mL) was added to a mixture of 1-dodecane-sulfonyl chloride (Maybridge) (0.8 g, 3.0 mmol) and 3-amino-4-methoxy-N-(3,4-dichloro-phenyl)-benzamide from Example 4 (0.73 g, 3.0 mmol) and stirred at room temperature. After 5 days the mixture was heated on a steambath for 1.5 hours, allowed to cool, and added to water (150 mL), acidified with 4N HCl, and stirred for an hour. The precipitate was filtered off, rinsed with water then with ethanol and dried to afford the product (1.3 g); m.p. 15-152° C. after recrystallization from ethanol and chromatography on silica gel in CHCl3/EtOAc (9:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06268387B1 |
| 出典データセット | uspto-grants-2001_07 |
| ORD ID | ord-83fc6643bd6247df8b62ee6a8338232d |
| 出典メモ | uspto-grants-2001_07 |