反応 #575723

ord-67b3606ed97745088224a32eb7d53c20

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to reflux for 48 hours
  2. 2
    その他The solvent is evaporated off under vacuum
  3. 3
    その他the residue is purified by chromatography on silica gel column (CH2Cl2/MeOH 60/40
  4. 4
    その他The product is obtained in the form of a white powder
  5. 5
    その他after precipitation from hexane

実験手順

1 g (1 equivalent) of α-chloroparatoluic acid and 1.22 mL (2 equivalents) of diethylamine are placed in solution in 30 mL of acetonitrile. The reaction mixture is taken to reflux for 48 hours. The solvent is evaporated off under vacuum and the residue is purified by chromatography on silica gel column (CH2Cl2/MeOH 60/40 then pure MeOH). The product is obtained in the form of a white powder after precipitation from hexane. (Yield=63%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06972343B1uspto-grants-2005_12