Reaktion #1884994

ord-a7ee0291405740d99c78f0dcbbe2ae71

Reaktionsgleichung

O=Cc1cccc(F)c1
3-fluoro benzaldehyde
O=C(O)CC(=O)O
malonic acid
C1CCNCC1
piperidine
c1ccncc1
pyridine
Cl
HCl
O=C(O)C=Cc1cccc(F)c1
3-fluoro-cinnamic acid
Ausbeute 84.0%

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter heating it to 80° C.
  2. 2
    workup.STIRRINGthe mixture was stirred for 12 hours
  3. 3
    SonstigeAfter the reaction
  4. 4
    Temperaturthe resulting solution cooled to room temperature
  5. 5
    FiltrationThe resulting powder was filtered
  6. 6
    Waschenwashed with water
  7. 7
    Sonstigedried in a vacuum oven

Vorschrift

5 g (40.1 mmol) of 3-fluoro benzaldehyde, 8.38 g (2 eq.) of malonic acid, and 0.34 g (0.1 eq.) of piperidine were added to 9.52 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 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: 84%)

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08343597B2uspto-grants-2013_01