反応 #5067

ord-c53f731d9de94323887be2d52a3919fc

反応条件

温度
-60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONWhen the addition
  2. 2
    workup.STIRRINGThe mixture is stirred for 2 hours at -40° C.
  3. 3
    workup.WAITfor 2 hours at ambient temperature before hydrolyzing using

実験手順

23.3 ml of a 1.6M solution of butyllithium in hexane are added dropwise to a solution, previously cooled to -60° C., of 8 g of 5-bromo-1,4-benzodioxane in 400 ml of tetrahydrofuran. When the addition is complete, the mixture is stirred at -60° C. for 5 minutes and a solution of 8 g of 1-benzylpiperid-4-one in 100 ml of tetrahydrofuran is then added dropwise. The mixture is stirred for 2 hours at -40° C. and then for 2 hours at ambient temperature before hydrolyzing using 80 ml of water.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05242933uspto-grants-1993_09