関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Thiophenol | HCID 7969 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Iodo-3-nitrobenzene | HCID 12574 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Nitro-3-(phenylsulfanyl)benzene | HCID 142232 | — |
反応手順
A mixture of thiophenol (1.0 g, 9.1 mmol), 3-iodonitrobenzene (1.9 g, 7.6 mmol), CuI (0.14 g, 0.76 mmol), K2CO3 (1.67 g, 12.1 mmol), and DMF (10 mL) was heated to 100° C. in a flame-dried sealed tube for 16 h. The mixture was allowed to cool and was poured over ice. The resulting mixture was extracted with EtOAc (2×), and the organic extracts were combined and washed sequentially with equal volumes of aqueous 1M HCl, water, and aqueous 1M NaOH. The solution was dried, concentrated, and the residue was purified by FCC (100:0 to 95:5 hexanes/EtOAc) to provide the titled compound, which was contaminated with ca. 10% thiophenol (1.43 g), and was taken on to subsequent steps without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08937078B2 |
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| 出典データセット | uspto-grants-2015_01 |
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| ORD ID | ord-0bcc46a1b38348919cfa06ce86502a56 |
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| 出典メモ | uspto-grants-2015_01 |
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