تفاعل #52883

ord-bf2446b1064144abbe0706083e973766

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 hydrogencarbonate solution and 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 (dichloromethane/methanol=50/1 to 10/1)

الإجراء التجريبي

218 mg (0.817 mmol) of 4-(3-chlorophenyl)-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylic acid and 126 mg (0.981 mmol) of 1-(3-aminopropyl)pyrrolidine were dissolved in 10 ml of DMF. 235 mg (1.23 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 hydrogencarbonate solution and 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 (dichloromethane/methanol=50/1 to 10/1) to obtain the title compound.

المصدر

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