化工社化工社 化学情報印刷レポート · 研究参考用
Water → 1-(Phenylethynyl)-4-(phenylsulfonyl)benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Iodobenzene | HCID 11575 | — |
| 反応物 | 4-Phenylsulfonylphenylethyne | HCID 19939320 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-(Phenylethynyl)-4-(phenylsulfonyl)benzene | HCID 21099403 | 28% |
反応手順
A mixture of 1-ethynyl-4-(phenylsulfonyl)benzene (100 mg, 0.4 mmol), iodobenzene (0.05 mL, 0.44 mmol) and triethylamine (1 mL) in toluene (1 mL) was degassed. Copper(I) iodide (3 mg, 0.004 mmol) and dichlorobis(triphenylphosphine)-palladium(II) (3 mg, 0.004 mmol) were added and the reaction stirred at room temperature overnight. The mixture was poured into water and extracted with ethyl acetate. The organic layer was dried and concentrated in vacuo. The residue was purified by preparative HPLC to give the title compound (35 mg, 28%). δH (500 MHz, d6 DMSO): 7.97 (4H, dd, J=2.6, 8.4 Hz), 7.77–7.69 (3H, m), 7.64–7.56 (4H, m), 7.43–7.41 (3H, m).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07217740B2 |
| 出典データセット | uspto-grants-2007_05 |
| ORD ID | ord-8973bec5db5f4dee8b621d09f2ec6299 |
| 出典メモ | uspto-grants-2007_05 |