反応 #5436

ord-4aeb686c490442b0b6a3ee76700a4b23

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮while saturating several times with gaseous methylamine
  2. 2
    その他The solvent is evaporated under reduced pressure

実験手順

4.5 g (11.5 mmols) of methyl 2-[[3-[4-(3-chlorophenyl)piperazin-1-yl]propyl]amino]pyrimidine-4-carboxylate and 200 ml of methanol are introduced into a 0.5 l, round bottomed flask and then the solution is saturated with gaseous methylamine. The reaction mixture is stirred at room temperature while saturating several times with gaseous methylamine. The solvent is evaporated under reduced pressure. 4.05 g (10.4 mmols) of base are obtained to which 104 ml of 0.1N hydrochloric acid in 2-propanol are added. The solvent is evaporated and the product is recrystallised from 2-butanone. 3.8 g of compound are obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05244894uspto-grants-1993_09