Ethyl Acetate → HCID 14370871, Verbindung
Reaktionsgleichung
[F:1][C:2]1[CH:8]=[C:7]([Br:9])[C:6]([O:10][C:11]([O:13][CH3:14])=[O:12])=[CH:5][C:3]=1[NH2:4].[C:15](OCC)(=[O:17])C>>[F:1][C:2]1[CH:8]=[C:7]([Br:9])[C:6]([O:10][C:11]([O:13][CH3:14])=[O:12])=[CH:5][C:3]=1[N:4]=[C:15]=[O:17]Komponenten
3
Reaktionsbedingungen
- Temperatur
- 80 °C
Versuchsvorschrift
A solution of trichloromethyl chloroformate trichloromethyl (15 ml, 125 mmol) in ethyl acetate was charged into a 500 ml-three neck flask equipped with a dropping funnel and distillation apparatus and, a solution of 2-fluoro-4-bromo-5-methoxycarbonyloxyaniline (28.0 g,113 mmol) in ethyl acetate (100 ml) was added dropwise over 20 minutes. After dropping, the mixture was heated at 80° C. and ethyl acetate was removed by distillation. After cooling, carbon tetrachloride (150 ml) was added and the undissolved substances were removed by filtration. The solvent was then removed from the filtrate by distillation under reduced pressure, whereby a brown solid of 2-fluoro-4-bromo-5-methoxycarbonyloxyphenyl isocyanate (29.1 g, yield 94%) was obtained.