반응 #1041

반응 방정식

i-propanol

4-bromo-3-chloro-3,4,4-trifluorobutanol

Jones reagent

→

4-bromo-3-chloro-3,4,4-trifluorobutanoic acid

수율 85.0%

4-bromo-3-chloro-3,4,4-trifiuorobutanoic acid

수율 85.0%

용매

methylene chloride

acetone

반응 조건

후처리

1. 1
   workup.STIRRINGThe mixture was then stirred at room temperature for 30 min
2. 2
   기타The precipitated salts were removed by filtration
3. 3
   세척washed with acetone
4. 4
   기타The residue obtained after concentration of the flitrate
5. 5
   세척washed with 1N HCl (50 mL), brine
6. 6
   건조dried over anhydrous magnesinm sulfate
7. 7
   기타Evaporation of the solvent

실험 절차

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.

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