反应详情

4-[5-Acetyl-3,6-dimethyl-2-oxo-1-(3-trifluoromethyl-phenyl)-1,2,3,4-tetrahydro-pyrimidin-4-yl]-3-bromo-benzonitrile (intermediate 4)(643.0 mg, 1.31 mmol), 1.1-bis(diphenyl-phosphino)-ferrocendichloropalladium(II), complex with dichloromethane (1:1) (51.5 mg, 0.06 mmol) and sodium acetate (327.5 mg, 4.0 mmol) are suspended in methanol (21 mL) and treated with carbon monoxide at 5 bar and 100° C. for 19 h. The reaction mixture is concentrated, water and ethyl acetate are added and the phases are separated. The organic phase is washed twice with water, dried over MgSO4 and concentrated. Yield: 671 mg. ESI mass spectrum: [M+H]+=472; Retention time HPLC: 1.12 min (HPLC method Z018_S04).

1. concentrationThe reaction mixture is concentrated
2. additionwater and ethyl acetate are added
3. customthe phases are separated
4. washThe organic phase is washed twice with water
5. dry with materialdried over MgSO4
6. concentrationconcentrated
7. custom1.12 min (HPLC method Z018_S04)