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Hydrochloric Acid → 3,4,4-Trifluoro-3-butenoic acid, 4-nitrophenyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Nitrophenol | HCID 980 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3,4,4-Trifluoro-3-butenoyl chloride | HCID 10920789 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 3,4,4-Trifluoro-3-butenoic acid, 4-nitrophenyl ester | HCID 15239190 | 92.1% |
反応手順
A solution of 4-nitrophenol (1.10 g, 0.0079 mole) and 3,4,4-trifluoro-3-butenoyl chloride (1.85 g, 0.0116 mole) in dry ether (15 mL) is treated dropwise with triethylamine (1.01 g, 0.01 mole) at -78° C. with stirring. The mixture is stirred at -78° C. for 10 min and allowed to reach room temperature. The reaction mixture is diluted with ether (20 mL), stirred with 15 mL of 2 N HCl. The organic layer is successively washed with water, 5% sodium bicarbonate, brine, and dried. The dark brown residue obtained after evaporation of the solvent was purified by passing through a short column of silica gel to give 1.9 g of the product as a brown solid, a 91% yield. m.p. 58°-62° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05623084 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-760aa76627d84edfb1a7dfe8d27792cc |
| 出典メモ | uspto-grants-1997_04 |