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Pyridine → 2-Oxo-2-(4-trifluoromethylphenyl)ethyl phenyl carbonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Phenyl chloroformate | HCID 15891 | — |
| 反応物 | 2-Hydroxy-1-[4-(trifluoromethyl)phenyl]ethan-1-one | HCID 11287169 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Oxo-2-(4-trifluoromethylphenyl)ethyl phenyl carbonate | HCID 12992962 | 53% |
反応手順
To a mixture of 2-hydroxy-4′-trifluoromethyl acetophenone (24.0 g), pyridine (10.3 g) and tetrahydrofuran (200 ml) was added dropwise phenyl chlorocarbonate (20.4 g) under ice-cooling, which was stirred at room temperature for 1 hour. The reaction mixture was concentrated, which was poured into water (500 ml), and extracted with ethyl acetate (150 ml×2). The organic layer was washed with water and then a saturated aqueous solution of sodium chloride, which was dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to crystallization by addition of isopropyl ether (100 ml) to give crystals of 2-oxo-2-(4-trifluoromethylphenyl)ethyl phenyl carbonate (18.9 g, 53%). Melting point 134-135° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06605629B1 |
| 出典データセット | uspto-grants-2003_08 |
| ORD ID | ord-e1d0f28c574a4582986d3542d7789975 |
| 出典メモ | uspto-grants-2003_08 |