تفاعل #52900

ord-783c753c13ee4c8cbc66bd363dbbb696

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةunder cooling with ice, and they
  2. 2
    تركيزAfter the concentration under reduced pressure
  3. 3
    workup.ADDITIONthe reaction mixture was diluted with ethyl acetate
  4. 4
    غسيلwashed with saturated aqueous sodium chloride solution
  5. 5
    تجفيفThe organic layer was dried over anhydrous magnesium sulfate
  6. 6
    تركيزconcentrated under reduced pressure
  7. 7
    أخرىThe residue was purified by the silica gel chromatography (hexane/ethyl acetate=2/1)

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06855716B2uspto-grants-2005_02