反応 #4748

ord-505171a282c949038b31467505f1365b

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The excess acrylonitrile is evaporated off under vacuum
  2. 2
    洗浄washed with 5% NaOH
  3. 3
    その他14.9 g (40% of theoretical) of a pale yellow oil is obtained in a sufficiently pure form for subsequent reactions

実験手順

28.7 g (0.15 mol) of 3-[(3-methylpyrrolidin-1-yl) methyl]phenol are heated under reflux together with 100 ml of acrylonitrile and 1.5 ml of 40% methanolic benzyltrimethylammonium hydroxide solution for 18 hours. The excess acrylonitrile is evaporated off under vacuum and the residue is taken up with ether, washed with 5% NaOH and reduced to the amine by reaction with 7.6 g (0.2 mol) of LiAlH4 in a manner analogous to Example 64 b. 14.9 g (40% of theoretical) of a pale yellow oil is obtained in a sufficiently pure form for subsequent reactions.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04727081uspto-grants-1988_02