Diethyl Ether → 1-Bromo-3,3-dimethyl-4-fluoro-2-butanone
Reaction equation
[Br:1]Br.[CH3:3][C:4]([CH3:10])([CH2:8][F:9])[C:5](=[O:7])[CH3:6].CCOCC>O>[Br:1][CH2:6][C:5](=[O:7])[C:4]([CH3:10])([CH3:3])[CH2:8][F:9]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
480 g of bromine were slowly added dropwise to a mixture of 354 g (3 mol) of 3,3-dimethyl-4-fluoro-butan-2-one and 2,000 ml of ether at 20° to 30° C., while cooling and stirring. The yellowish solution was subsequently stirred, at 20° C., for a further 1 hour and 500 ml of water were then added carefully. 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% theory) of 1-bromo-3,3-dimethyl-4-fluoro-butan-2-one of boiling point 80°-90° C./11 mm Hg were obtained. ##STR24##
Workup
- temperaturewhile cooling
- stirringThe yellowish solution was subsequently stirred, at 20° C., for a further 1 hour
- customThe ether phase was separated off
- washwashed several times with water
- dry with materialdried over sodium sulphate
- distillationAfter distilling off the solvent
- distillationthe residue was distilled under a waterpump vacuum
Sources & evidence
- ORD record
- ord-cd9b21c646cb41da9b3e24b31e7fbd77
- Source dataset
- uspto-grants-1983_05
- Patent number
- US04382944
Reaction notes
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