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Ici 222155 → 1-[3,5-Dimethyl-4-[(nitromethyl)sulphonyl]phenyl]-3-[(2-methylphenyl)sulphonyl]urea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ici 222155 | HCID 195716 | — |
| 反応物 | o-Toluenesulfonyl Isocyanate | HCID 2733313 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-[3,5-Dimethyl-4-[(nitromethyl)sulphonyl]phenyl]-3-[(2-methylphenyl)sulphonyl]urea | HCID 18676541 | 86% |
反応手順
A solution of 0.77 ml (5.09 mmol) of o-toluenesulphonyl isocyanate in 7.7 ml of anhydrous methylene chloride is added dropwise to a suspension, maintained under a nitrogen atmosphere, of 1.3 g (5.32 mmol) of 3,5-dimethyl-4-[(nitromethyl)sulphonyl]aniline in 25.6 ml of anhydrous methylene chloride. The temperature of the reaction medium rises spontaneously by 7° C. A precipitate forms in the solution initially obtained. Stirring is continued for 1 hour at room temperature and the solid is then isolated by filtration and washed with hexane to give 1.9 g (yield=86%) of 1-[3,5-dimethyl-4-[(nitromethyl)sulphonyl]phenyl]-3-[(2-methylphenyl)sulphonyl]urea.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06509499B1 |
| 出典データセット | uspto-grants-2003_01 |
| ORD ID | ord-eb98b86be4084b87bec67089f8d78ed8 |
| 出典メモ | uspto-grants-2003_01 |