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异丙醇 → 4-Bromo-3-chloro-3,4,4-trifluorobutanoic acid
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 异丙醇 | HCID 3776 | — |
| 反应物 | 4-Bromo-3-chloro-3,4,4-trifluorobutan-1-ol | HCID 21836477 | — |
| 反应物 | Jones' reagent | HCID 131709961 | — |
| 溶剂 | 丙酮 | HCID 180 | — |
| 溶剂 | 二氯甲烷 | HCID 6344 | — |
| 产物 | 4-Bromo-3-chloro-3,4,4-trifluorobutanoic acid | HCID 10912127 | 85% |
反应步骤
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 filtrate was dissolved in methylene chloride (100 mL), washed with 1N HCl (50 mL), brine, and dried over anhydrous magnesium 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.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US05514717 |
| 来源数据集 | uspto-grants-1996_05 |
| ORD ID | ord-77eaa78347e14d699c10a4101f11b5b8 |
| 来源说明 | uspto-grants-1996_05 |