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聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 1-(Phenylethynyl)-4-(phenylsulfonyl)benzene
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 反应物 | 三乙胺 | HCID 8471 | — |
| 反应物 | 碘苯 | HCID 11575 | — |
| 反应物 | 4-Phenylsulfonylphenylethyne | HCID 19939320 | — |
| 催化剂 | 碘化亚铜 | HCID 24350 | — |
| 催化剂 | HCID 178418476 | HCID 178418476 | — |
| 溶剂 | 甲苯 | HCID 1140 | — |
| 产物 | 1-(Phenylethynyl)-4-(phenylsulfonyl)benzene | HCID 21099403 | 28% |
反应步骤
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).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US07217740B2 |
| 来源数据集 | uspto-grants-2007_05 |
| ORD ID | ord-8973bec5db5f4dee8b621d09f2ec6299 |
| 来源说明 | uspto-grants-2007_05 |