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Isopropanol → 4-Bromo-3-chloro-3,4,4-trifluorobutanoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | 4-Bromo-3-chloro-3,4,4-trifluorobutan-1-ol | HCID 21836477 | — |
| 反応物 | Jones' reagent | HCID 131709961 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Bromo-3-chloro-3,4,4-trifluorobutanoic acid | HCID 10912127 | 85% |
反応手順
A solution of 4-bromo-3-chloro-3,4,4-trifluorobutanol (IX) (2.41 g, 10 mmol) in acetone (35 mL) was treated with Jones reagent (7.5 mL) in 10 min with stirring and cooling (ice-water bath). The mixture was then stirred at room temperature for 30 min and 0.5 mL of i-propanol was then added. The precipitated salts were removed by filtration, washed with acetone. The residue obtained after concentration of the flitrate was dissolved in methylene chloride (100 mL), washed with 1N HCl (50 mL), brine, and dried over anhydrous magnesinm sulfate. Evaporation of the solvent gave 2.17 g (85%) of 4-bromo-3-chloro-3,4,4-trifluorobutanoic acid (VIII) as a clear oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05723470 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-cc001eb75d5743259d85df36a16ea38b |
| 出典メモ | uspto-grants-1998_03 |