Isopropanol → 4-Bromo-3-chloro-3,4,4-trifluorobutanoic acid

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.

1. stirringThe mixture was then stirred at room temperature for 30 min
2. customThe precipitated salts were removed by filtration
3. washwashed with acetone
4. customThe residue obtained after concentration of the filtrate
5. washwashed with 1N HCl (50 mL), brine
6. dry with materialdried over anhydrous magnesium sulfate
7. customEvaporation of the solvent

ORDレコード

ord-77eaa78347e14d699c10a4101f11b5b8

出典データセット

uspto-grants-1996_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05514717