反应 #156301

ord-72974516ebbc4ed798d741834e8fb5e2

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩The reaction mixture was concentrated under reduced pressure
  2. 2
    workup.ADDITIONto the residue were added a saturated aqueous sodium hydrogen carbonate solution and ethyl acetate
  3. 3
    其他the aqueous layer was separated
  4. 4
    洗涤The organic layer was washed with saturated brine
  5. 5
    干燥dried over anhydrous magnesium sulfate
  6. 6
    其他the solvent was evaporated under reduced pressure
  7. 7
    其他The residue was purified by basic silica gel column chromatography (chloroform/methanol)

实验过程

To a solution of 2.0 g of tert-butyl 4-[(cyclopropyloxy)methyl]piperidine-1-carboxylate in 20 mL of dichloromethane was added 3.0 mL of trifluoroacetic acid, followed by stirring at room temperature for 2 hours. The reaction mixture was concentrated under reduced pressure, and to the residue were added a saturated aqueous sodium hydrogen carbonate solution and ethyl acetate, and then the aqueous layer was separated. The organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by basic silica gel column chromatography (chloroform/methanol) to obtain 756 mg of 4-[(cyclopropyloxy)methyl]piperidine.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08822448B2uspto-grants-2014_09