関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4,4,5,5-Tetramethyl[1,3,2]dioxaborolane | HCID 2734768 | — |
| 反応物 | 3'-Bromo-2,2,2-trifluoroacetophenone | HCID 14647442 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 生成物 | 2,2,2-Trifluoro-1-(3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-YL)phenyl)ethanol | HCID 21886155 | 53% |
反応手順
To an oven-dried round bottom flask fitted with a stir bar and a rubber septum was added 1-(3-bromo-phenyl)-2,2,2-trifluoro-ethanone (560 mg, 2.2 mmol, as prepared in Example 28, step a), 4,4,5,5-tetramethyl-[1,3,2]dioxaborolane (0.96 mL, 6.6 mmol, Aldrich Chemical Company), (PPh3)2PdCl2 (93 mg, 0.132 mmol, Strem Chemicals, Inc., Newburyport, Mass.), and Et3N (1.8 mL, 13.2 mmol). The reaction mixture was evacuated, purged with argon, and then suspended in dioxane (16 mL). After stirring for 18 hr at 95° C., the reaction was allowed to cool and then filtered through Celite.® The filtrate was concentrated in vacuo and the residue was purified by chromatography (SiO2, flash elution: 5% EtOAc in hexanes) to give 350 mg (53%) of an oil that was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07109354B2 |
|---|
| 出典データセット | uspto-grants-2006_09 |
|---|
| ORD ID | ord-1c111f7200ef44e287b880dfd8f2178d |
|---|
| 出典メモ | uspto-grants-2006_09 |
|---|