反应详情

4-(2-Bromo-4-cyano-phenyl)-3,6-dimethyl-2-oxo-1-(3-trifluoromethyl-phenyl)-1,2,3,4-tetrahydro-pyrimidine-5-carboxylic acid ethyl ester (intermediate 8, 7.16 g, 13.7 mmol), 1.1-bis(diphenylphosphino)-ferrocendichloropalladium(H), complex with dichloromethane (1:1) (559.3 mg, 0.69 mmol) and sodium acetate (3.37 g, 41.1 mmol) are suspended in methanol (120 mL) and treated with carbon monoxide at 8 bar and 100° C. for 19 h. A small amount of 1.1-bis(diphenylphosphino)-ferrocendichloropalladium(II), complex with dichloromethane (1:1) is added and the reaction under carbon monoxide is continued at 8 bar and 100° C. for 19 h. The reaction mixture is concentrated and purified by reversed phase HPLC. Yield: 3.70 g. ESI mass spectrum: [M+H]+=502; Retention time HPLC: 1.20 min (HPLC method Z018_S04)

1. customthe reaction under carbon monoxide
2. concentrationThe reaction mixture is concentrated
3. custompurified by reversed phase HPLC
4. custom1.20 min (HPLC method Z018_S04)