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Triethylamine → 3-(4-Hydroxy-3-fluorophenyl)-acrylic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl Acrylate | HCID 8821 | — |
| 反応物 | Tri-o-tolylphosphine | HCID 80271 | — |
| 反応物 | 4-Bromo-2-fluorophenol | HCID 2724981 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-(4-Hydroxy-3-fluorophenyl)-acrylic acid ethyl ester | HCID 54033199 | — |
反応手順
A solution of 2-fluoro-4-bromophenol 15-1 (50 g, 261.8 mmol), ethyl acrylate (34 mL), Pd(OAc)2 (2.5 g), tri-o-tolylphosphine (5 g) and triethylamine (83 mL) was heated to 100° C. in a sealed tube for 12 h. The reaction was cooled to room temperature and diluted with dichloromethane (100 mL). The organic solution was washed with 10% aq. citric acid (40 mL), satd aq NaHCO3, and brine (40 mL). The organic solution was dried over MgSO4, filtered and concentrated. The residue was purified by flash chromatography (50:50 hexanes/EtOAc to 100% EtOAc) to give acrylic acid 15-2 as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06066648 |
| 出典データセット | uspto-grants-2000_05 |
| ORD ID | ord-95e7ea1780ef4d6e96914cb0744ea71c |
| 出典メモ | uspto-grants-2000_05 |