Triethylamine → 2,4-difluorophenyl ethyl carbonate
Reaction equation
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[OH:9].C(N(CC)CC)C.Cl[C:18]([O:20][CH2:21][CH3:22])=[O:19]>ClCCl>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[O:9][C:18]([O:20][CH2:21][CH3:22])=[O:19]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
104 g (796 mmol) of 2,4-difluorophenol was dissolved in 800 ml of dichloromethane, 132 ml of triethylamine and 92.0 ml of ethyl chloroformate were added under ice-cooling and the mixture was stirred at -10° to 0° C. for 2 hours. The reaction solution was washed with an aqueous saturated solution of sodium chloride and dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure to give 156 g (97%) of 2,4-difluoro-O-ethoxycarbonylphenol.
Workup
- temperaturecooling
- washThe reaction solution was washed with an aqueous saturated solution of sodium chloride
- dry with materialdried over anhydrous magnesium sulfate
- distillationthe solvent was distilled off under reduced pressure
Sources & evidence
- ORD record
- ord-af20c829270846fc8ee7fbf569350521
- Source dataset
- uspto-grants-1996_07
- Patent number
- US05539112
Reaction notes
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