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Triethylamine → N-[4-(5-chloro-2-pyrimidinyloxy)-3-methylphenyl]-2-nitrobenzenesulfenamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2-Nitrobenzenesulfenyl chloride | HCID 24319 | — |
| 反応物 | 4-((5-Chloropyrimidin-2-yl)oxy)-3-methylaniline | HCID 14207808 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N-[4-(5-chloro-2-pyrimidinyloxy)-3-methylphenyl]-2-nitrobenzenesulfenamide | HCID 10000368 | 83.6% |
反応手順
2.0 g of 4-(5 chloro-2-pyrimidinyloxy)-3methylaniline and 0.94 g of triethylamine were dissolved in 20 ml of toluene, and a solution of 1.61 g of 2-nitrobenzenesulfenyl chloride dissolved in 5 ml of toluene was dropwise added thereto at room temperature. The mixture was reacted at room temperature for 1 hour under stirring. After completion of the reaction, ethyl acetate was added to the reaction product, and the ethyl acetate layer was washed with water, dried over Glauber's salt and then purified by column chromatography to obtain 2.76 g of N-[4-(5-chloro-2-pyrimidinyloxy)-3-methylphenyl]-2-nitrobenzenesulfenamide (Intermediate Compound No. 37) (melting point: 74°-85° C.) in a yellow non-crystalline form.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04987135 |
| 出典データセット | uspto-grants-1991_01 |
| ORD ID | ord-635377d9a71e459093799c5dc60a7731 |
| 出典メモ | uspto-grants-1991_01 |