Reaktion #52883

Reaktionsgleichung

4-(3-chlorophenyl)-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylic acid

1-(3-aminopropyl)pyrrolidine

WSC hydrochloride

→

title compound

4-(3-chlorophenyl)-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylic acid (3-pyrrolidine-1-yl-propyl)amide

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder cooling with ice, and they
2. 2
   EinengenAfter the concentration under reduced pressure
3. 3
   workup.ADDITIONthe reaction mixture was diluted with ethyl acetate
4. 4
   Waschenwashed with saturated aqueous sodium hydrogencarbonate solution and saturated aqueous sodium chloride solution
5. 5
   TrocknenThe organic layer was dried over anhydrous magnesium sulfate
6. 6
   Einengenconcentrated under reduced pressure
7. 7
   SonstigeThe residue was purified by the silica gel chromatography (dichloromethane/methanol=50/1 to 10/1)

Vorschrift

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.

Quelle