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Sodium hydride → 2,2,2-Trifluoro-1-(4-fluorophenyl)ethyl trifluoromethanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Trifluoromethanesulfonyl chloride | HCID 79000 | — |
| 反応物 | 2,2,2-Trifluoro-1-(4-fluorophenyl)ethanol | HCID 11148246 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 2,2,2-Trifluoro-1-(4-fluorophenyl)ethyl trifluoromethanesulfonate | HCID 57562097 | 101.2% |
反応手順
NaH (640 mg, 16 mmol, 60% in mineral oil) was washed twice with hexane (20 mL) and then suspended in dried diethyl ether (20 mL). A solution of 2,2,2-trifluoro-1-(4-fluoro-phenyl)ethanol (1.94 g, 10 mmol) in diethyl ether (10 mL) was added at 0° C. After stirring for 2 h at room temperature, a solution of trifluoromethanesulfonyl chloride (1.68 g, 10 mmol) in diethyl ether (10 mL) was added. After 2 h, the reaction mixture was quenched by adding a solution of NaHCO3 and the product was extracted with diethyl ether. The extracts were washed with brine and dried, and the solvent was removed to yield trifluoromethanesulfonic acid 2,2,2-trifluoro-1-(4-fluorophenyl)ethyl ester (3.3 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07737300B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-28c59b0678af4521a6e78ceace972cf5 |
| 出典メモ | uspto-grants-2010_06 |