Реакция #52900

ord-783c753c13ee4c8cbc66bd363dbbb696

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураunder cooling with ice, and they
  2. 2
    КонцентрированиеAfter the concentration under reduced pressure
  3. 3
    workup.ADDITIONthe reaction mixture was diluted with ethyl acetate
  4. 4
    Промывкаwashed with saturated aqueous sodium chloride solution
  5. 5
    СушкаThe organic layer was dried over anhydrous magnesium sulfate
  6. 6
    Концентрированиеconcentrated under reduced pressure
  7. 7
    ДругоеThe residue was purified by the silica gel chromatography (hexane/ethyl acetate=2/1)

Методика

158 mg (0.563 mmol) of 4-(3-chlorophenyl)-2-methoxy-6-methyl-1,4-dihydropyrimidine-5-carboxylic acid and 178 mg (0.844 mmol) of 3,3-diphenylpropylamine were dissolved in 20 ml of dichloromethane. 162 mg (0.844 mmol) of WSC hydrochloride was added to the obtained solution under cooling with ice, and they were stirred at room temperature overnight. After the concentration under reduced pressure, the reaction mixture was diluted with ethyl acetate and then washed with saturated aqueous sodium chloride solution. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by the silica gel chromatography (hexane/ethyl acetate=2/1) to obtain the title compound.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06855716B2uspto-grants-2005_02