反应详情

139 mg (0.417 mmol) of 6-(2-chloroethoxymethyl)-4-(3-chlorophenyl)-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylic acid and 106 mg (0.500 mmol) of 3,3-diphenylpropylamine were dissolved in 10 ml of dichloromethane. 120 mg (0.626 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 1 N hydrochloric acid, 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 obtain the title compound.

1. temperatureunder cooling with ice, and they
2. concentrationAfter the concentration under reduced pressure
3. additionthe reaction mixture was diluted with ethyl acetate
4. washwashed with 1 N hydrochloric acid, saturated aqueous sodium hydrogencarbonate solution and saturated aqueous sodium chloride solution
5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by the silica gel chromatography (dichloromethane/methanol=50/1)