反应 #52874

反应方程式

1-hydroxybenzotriazole

4-(3-chlorophenyl)-6-[(2-cyclohexylethoxy)methyl]-2-phenyl-1,4-dihydropyrimidine-5-carboxylic acid

3,3-diphenylpropylamine

HOBT

WSC hydrochloride

→

title compound

4-(3-chlorophenyl)-6-[(2-cyclohexylethoxy)methyl]-5-(3,3-diphenylpropylcarbamoyl)-2-phenyl-1,4-dihydropyrimidine

溶剂

dichloromethane

dichloromethane

反应条件

后处理

1. 1
   workup.ADDITIONwere added to the obtained solution
2. 2
   温度under cooling with ice, and they
3. 3
   洗涤washed with saturated aqueous sodium hydrogencarbonate solution
4. 4
   干燥The organic layer was dried over anhydrous sodium sulfate
5. 5
   浓缩concentrated under reduced pressure
6. 6
   其他The residue was purified by the silica gel chromatography (hexane/ethyl acetate=3/1 to 1/1)

实验过程

60.0 mg (0.110 mmol) of 4-(3-chlorophenyl)-6-[(2-cyclohexylethoxy)methyl]-2-phenyl-1,4-dihydropyrimidine-5-carboxylic acid and 34.9 mg (0.165 mmol) of 3,3-diphenylpropylamine were dissolved in 10 ml of dichloromethane. 31.6 mg (0.165 mmol) of WSC hydrochloride and 16.8 mg (0.110 mmol) of 1-hydroxybenzotriazole (hereinafter referred to as “HOBT”) were added to the obtained solution under cooling with ice, and they were stirred at room temperature overnight. The reaction mixture was diluted with dichloromethane and then washed with saturated aqueous sodium hydrogencarbonate solution. The organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was purified by the silica gel chromatography (hexane/ethyl acetate=3/1 to 1/1) to obtain the title compound.

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