Reaktion #1929004

ord-c1925dd40e52442f900efa79d41ae04f

Reaktionsgleichung

FC(F)(F)c1ccc(N2CCC(Br)CC2)nc1
compound ( 48 )
FC(F)(F)c1ccc(N2CCC(Br)CC2)nc1
4-bromo-1-[5-(trifluoromethyl)-2-pyridyl]piperidine
[H-].[Na+]
sodium hydride
CN(C)C=O
DMF
CCCOc1cc(C(F)(F)F)ccc1S
compound ( 46 )
CCCOc1cc(C(F)(F)F)ccc1S
2-propoxy-4-(trifluoromethyl)benzenethiol
CCCOc1cc(C(F)(F)F)ccc1SC1CCN(c2ccc(C(F)(F)F)cn2)CC1
4-[2-propoxy-4-(trifluoromethyl)phenylsulfanyl]-1-[5-(trifluoromethyl)-2-pyridyl]piperidine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated to 100° C.
  2. 2
    workup.STIRRINGwas then stirred for 1 hour
  3. 3
    TemperaturAfter the mixture was cooled
  4. 4
    Extraktionwas then subjected to extraction with ethyl acetate
  5. 5
    WaschenAfter its organic layer was washed with water
  6. 6
    Trocknenwas then dried with anhydrous magnesium sulfate, it
  7. 7
    Filtrationwas filtered
  8. 8
    Einengenwas then concentrated under reduced pressure
  9. 9
    SonstigeIts residue was purified by column chromatography
  10. 10
    Sonstigeto produce the chemical compound

Vorschrift

After 60% sodium hydride was added, with chilling on ice, to the DMF (7 ml) solution of the chemical compound (46) (0.62 g), it was warmed to room temperature, and was then stirred for 30 minutes. After the chemical compound (48) (0.74 g) was added to the mixture, it was heated to 100° C., and was then stirred for 1 hour. After the mixture was cooled, it was poured into water, and was then subjected to extraction with ethyl acetate. After its organic layer was washed with water, and was then dried with anhydrous magnesium sulfate, it was filtered, and was then concentrated under reduced pressure. Its residue was purified by column chromatography to produce the chemical compound mentioned in the above title (0.90 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: USRE045364E1uspto-grants-2015_02