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Dimethyl Sulfoxide → HCID 85787323、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Perfluorooctyl iodide | HCID 10491 | — |
| 反応物 | Benzene, 1-iodo-4-(trifluoromethyl)- | HCID 67993 | — |
| 触媒 | 2,2'-Bipyridine | HCID 1474 | — |
| 触媒 | Copper | HCID 23978 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 85787323 | HCID 85787323 | 90.2% |
反応手順
A solution of C8F17I (12 g, 22 mmol) was added dropwise over 10 min to a stirred mixture of 4-iodobenzotrifluoride (3 g, 11 mmol), copper powder (5.6 g, 0.088 mmol), 2,2′-bipyridine (120 mg, 0.8 mmol), DMSO (30 mL) at 70° C. The reaction mixture was subsequently stirred for a further 72 h at this temperature. After cooling to room temperature, it was poured into a beaker containing ether (100 mL) and water (100 mL). After filtering, the organic layer was separated, washed with water (3×50 mL) and dried over MgSO4. Sublimation gave the product 10 as a white solid (5.6 g, 90%): 1H NMR (300 MHz, CDCl3): 7.77 (4H, dd, J=8.1 and 8.4 Hz); 19F NMR (282 MHz, CDCl3): −64.0, −81.4, −111.6, −121.4, −122.0, −122.1, −122, 9, −126, 3.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07700366B2 |
| 出典データセット | uspto-grants-2010_04 |
| ORD ID | ord-35dd165bd3564dea86d6ecab631844d9 |
| 出典メモ | uspto-grants-2010_04 |