反応 #52901

ord-7af937a590974f16ad36907baa32ed2e

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他An insoluble matter thus formed
  2. 2
    ろ過was filtered out
  3. 3
    濃縮the filtrate was concentrated under reduced pressure
  4. 4
    その他The residue was purified by the basic silica gel chromatography (100% dichloromethane)

実験手順

111 mg (0.234 mmol) of 4-(3-chlorophenyl)-2-methoxyl-6-methyl-1,4-dihydropyrimidine-5-carboxylic acid (3,3-diphenylpropyl)amide was dissolved in 5 ml of ethanol. 67.4 mg (0.702 mmol) of ammonium carbonate and 11.8 mg (0.187 mmol) of ammonium acetate were added to the obtained solution, and they were stirred at 80° C. for 2 days. The reaction mixture was diluted with ethyl acetate. An insoluble matter thus formed was filtered out, and the filtrate was concentrated under reduced pressure. The residue was purified by the basic silica gel chromatography (100% dichloromethane) to obtain the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06855716B2uspto-grants-2005_02