Reaktion #1884996

ord-7c9346e13d804a15b62d90ced5b74de8

Reaktionsgleichung

O=Cc1c(F)c(F)c(F)c(F)c1F
pentafluoro-benzaldehyde
O=C(O)CC(=O)O
malonic acid
C1CCNCC1
piperidine
c1ccncc1
pyridine
Cl
HCl
O=C(O)C=Cc1c(F)c(F)c(F)c(F)c1F
Pentafluoro-Cinnamic Acid
Ausbeute 13.0%

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 was cooled down to room temperature
  5. 5
    FiltrationThe resulting powder was filtered
  6. 6
    Waschenwashed with water
  7. 7
    Sonstigedried in a vacuum oven

Vorschrift

20 g (42 mmol) of pentafluoro-benzaldehyde, 21.23 g (2 eq.) of malonic acid, and 0.85 g (0.1 eq.) of piperidine were added to 24 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 was 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: 13%)

Quelle

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