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 then 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. 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 (yield assumed to be quantitive).

1. customThe solvent is then 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 (yield assumed to be quantitive)