反应 #1929004

ord-c1925dd40e52442f900efa79d41ae04f

反应方程式

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

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated to 100° C.
  2. 2
    workup.STIRRINGwas then stirred for 1 hour
  3. 3
    温度After the mixture was cooled
  4. 4
    萃取was then subjected to extraction with ethyl acetate
  5. 5
    洗涤After its organic layer was washed with water
  6. 6
    干燥was then dried with anhydrous magnesium sulfate, it
  7. 7
    过滤was filtered
  8. 8
    浓缩was then concentrated under reduced pressure
  9. 9
    其他Its residue was purified by column chromatography
  10. 10
    其他to produce the chemical compound

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE045364E1uspto-grants-2015_02