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Triethylamine → 4-Methoxy-2',4',6'-tri-iso-propylbiphenyl
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,3,5-Triisopropylbenzene | HCID 12860 | — |
| 反応物 | (4-Methoxyphenyl)boronic acid | HCID 201262 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | 4-Methoxy-2',4',6'-tri-iso-propylbiphenyl | HCID 15467666 | 88.3% |
反応手順
4-Methoxyphenylboronic acid (152 mg, 1.00 mmol), and Pd(dtbpf)Cl2 (6 mg, 0.01 mmol) were added to a reaction tube equipped with a magnetic stir bar. Under a positive flow of argon while stirring, surfactant solution (1.0 mL, 2 wt % TPGS-M-PEG-750 in water), 2,4,6-triisopropylbenzene (126 μL, 0.50 mmol), and Et3N (0.21 mL, 1.5 mmol) were added by syringe and stirred vigorously for 24 h. The reaction mixture was then diluted with brine and extracted with EtOAc. The solution obtained was dried over MgSO4 and concentrated by rotary evaporation. The residue was purified by flash column chromatography eluting with 5% CH2Cl2/hexanes to afford the product (137 mg, 88%) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08785665B2 |
| 出典データセット | uspto-grants-2014_07 |
| ORD ID | ord-0ee23a9e93d6404f995cfad26ddfcd72 |
| 出典メモ | uspto-grants-2014_07 |