反应详情

Palladium on carbon (10%) was added to a solution of 1660 mg (7.0 mmol) of tert-butyl (2E)-3-(3-amino-2-fluorophenyl)acrylate in a mixture of 5 ml of ethanol and 3 ml of THF, and the mixture was stirred vigorously at atmospheric pressure under an atmosphere of hydrogen overnight. The reaction mixture was then filtered through kieselguhr and the filter residue was washed repeatedly with ethanol/THF. The combined filtrates were concentrated under reduced pressure and the residue was purified by chromatography on silica gel (mobile phase cyclohexane/ethyl acetate 20:1→10:1). This gave 1350 mg of the target product (80.6% of theory).

1. filtrationThe reaction mixture was then filtered through kieselguhr
2. washthe filter residue was washed repeatedly with ethanol/THF
3. concentrationThe combined filtrates were concentrated under reduced pressure
4. customthe residue was purified by chromatography on silica gel (mobile phase cyclohexane/ethyl acetate 20:1→10:1)