Reaktion #1884995
ord-6ae797dfaf714ea596086c22c9298f6b
Reaktionsgleichung
3,4-di-fluoro-benzaldehyde
malonic acid
piperidine
pyridine
HCl
→
3,4-di-fluoro-cinnamic acid
Ausbeute 95.0%
Reagenzien
Keine
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturAfter heating it to 80° C.
- 2workup.STIRRINGthe mixture was stirred for 12 hours
- 3SonstigeAfter the reaction
- 4Temperaturthe resulting solution cooled down to room temperature
- 5FiltrationThe resulting powder was filtered
- 6Waschenwashed with water
- 7Sonstigedried in a vacuum oven
Vorschrift
10 g (70.4 mmol) of 3,4-di-fluoro-benzaldehyde, 14.65 g (2 eq.) of malonic acid, and 0.59 g (0.1 eq.) of piperidine were added to 16.7 g (3 eq.) of pyridine and stirred at room temperature for about 1 hour. After heating it to 80° C., the mixture was stirred for 12 hours. After the reaction, the resulting solution cooled down to room temperature and was slowly added with 1M HCl until it was titrated to about pH 4. The resulting powder was filtered and washed with water, and then dried in a vacuum oven. (Yield: 95%)