Réaction #1884995

Équation de réaction

3,4-di-fluoro-benzaldehyde

malonic acid

piperidine

pyridine

HCl

→

3,4-di-fluoro-cinnamic acid

Rendement 95.0%

Conditions de réaction

Traitement

1. 1
   TempératureAfter heating it to 80° C.
2. 2
   workup.STIRRINGthe mixture was stirred for 12 hours
3. 3
   AutreAfter the reaction
4. 4
   Températurethe resulting solution cooled down to room temperature
5. 5
   FiltrationThe resulting powder was filtered
6. 6
   Lavagewashed with water
7. 7
   Autredried in a vacuum oven

Mode opératoire

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%)

Source