반응 #1929004

ord-c1925dd40e52442f900efa79d41ae04f

반응 방정식

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

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated to 100° C.
  2. 2
    workup.STIRRINGwas then stirred for 1 hour
  3. 3
    온도After the mixture was cooled
  4. 4
    추출was then subjected to extraction with ethyl acetate
  5. 5
    세척After its organic layer was washed with water
  6. 6
    건조was then dried with anhydrous magnesium sulfate, it
  7. 7
    여과was filtered
  8. 8
    농축was then concentrated under reduced pressure
  9. 9
    기타Its residue was purified by column chromatography
  10. 10
    기타to produce the chemical compound

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: USRE045364E1uspto-grants-2015_02