反応 #156294

ord-2390eb3d0a4647d3b0b617a4197dcc83

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGstirring at 75° C. for 2 days
  2. 2
    ろ過The reaction mixture was filtered through celite
  3. 3
    濃縮the filtrate was concentrated under reduced pressure
  4. 4
    その他The residue was purified by silica gel column chromatography (n-hexane/ethyl acetate)

実験手順

4.3 g of tert-butyl 4-(hydroxymethyl)piperidine-1-carboxylate, 66 mg of 4,7-diphenyl-1,10-phenanthroline, and 45 mg of palladium acetate were added to 50 mL of butylvinyl ether, followed by stirring at room temperature for 15 minutes, and stirring at 75° C. for 2 days. The reaction mixture was filtered through celite, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane/ethyl acetate) to obtain 4.4 g of tert-butyl 4-[(vinyloxy)methyl]piperidine-1-carboxylate.

出典

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