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Hydrochloric Acid → 4-(4-Amino-phenylsulfanyl)-N-(4-bromo-phenyl)-3-nitro-benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 4-Aminothiophenol | HCID 14510 | — |
| 反応物 | N-(4-bromophenyl)-4-chloro-3-nitrobenzamide | HCID 1068537 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(4-Amino-phenylsulfanyl)-N-(4-bromo-phenyl)-3-nitro-benzamide | HCID 67040850 | 96% |
反応手順
A solution of the product from Example 10A (3.0 g, 8.44 mmol), 4-aminothiophenol (1.06 g, 8.44 mmol) and cesium carbonate (5.5 g, 17.0 mmol) in N,N-dimethylformamide (15 mL) was heated to 90° C. for 4 hours. After cooling to room temperature the mixture was poured into ice water (100 mL) and the resultant solution acidified to pH 5 with 1N aqueous hydrochloric acid. The solution was then extracted with ethyl acetate (3×50 mL), the combined extracts dried over sodium sulfate, filtered and concentrated under vacuum to provide the title compound as an orange solid (3.6 g, 96%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07910595B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-267650fa143b451f829bc3cb6156fe0a |
| 出典メモ | uspto-grants-2011_03 |