反应详情

2.00 g (5.79 mmol) of ethyl 3-oxo-3-(2,4,5-trifluoro-3-methoxyphenyl)propanoate (for preparation see Journal of Medicinal Chemistry (1995), 38 (22), 4478-87) are stirred under reflux in 3.8 ml (4.14 g, 40.55 mmol) of acetic anhydride and 4.82 ml (4.29 g, 28.96 mmol) of triethyl orthoformate for 2 h. The solvent is subsequently removed completely on a rotary evaporator and the residue is dissolved in 10 ml of ethanol. 1.03 g (10.43 mmol) of 2,2,2-trifluoro-1-aminoethane are added dropwise to the ice-cooled solution, and the mixture is brought to room temperature and stirred at that temperature overnight. For the work-up, the solvent is removed and the residue is reacted further as a crude product without purification steps.

1. customThe solvent is subsequently removed completely on a rotary evaporator
2. dissolutionthe residue is dissolved in 10 ml of ethanol
3. temperaturecooled solution
4. customis brought to room temperature
5. customFor the work-up, the solvent is removed
6. customthe residue is reacted further as a crude product without purification steps