Diethyl Ether → 1-Bromo-3,3-dimethyl-4-fluoro-2-butanone

480 g of bromine were slowly added dropwise to a mixture of 354 g (3 mols) of 3,3-dimethyl-4-fluoro-2-butanone and 2,000 ml of ether at 20° to 30° C., while cooling and stirring. The yellowish solution was subsequently stirred for a further hour at 20° C. and 500 ml of water were then carefully added. The ether phase was separated off, washed several times with water and dried over sodium sulphate. After distilling off the solvent, the residue was distilled under a waterpump vacuum. 472 g (80% of theory) of 1-bromo-3,3-dimethyl-4-fluoro-2-butanone of boiling point 80°-90° C./11 mm Hg were obtained. ##STR81##

1. temperaturewhile cooling
2. stirringThe yellowish solution was subsequently stirred for a further hour at 20° C.
3. customThe ether phase was separated off
4. washwashed several times with water
5. dry with materialdried over sodium sulphate
6. distillationAfter distilling off the solvent
7. distillationthe residue was distilled under a waterpump vacuum

ORD record

ord-c15c99c0efeb4258b92aff0d9b95adf0

Source dataset

uspto-grants-1983_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04415586