反应详情

Methyliodide (c=2 mol/L, 1.1 mL, 17.7 mmol) is added to a solution 4-(2-Bromo-4-cyano-phenyl)-6-methyl-2-oxo-1-(3-trifluoromethyl-phenyl)-1,2,3,4-tetrahydro-pyrimidine-5-carboxylic acid ethyl ester (intermediate 7. 47 g, 14.7 mmol) and cesium carbonate (7.9 g, 24.3 mmol) in N,N-dimethylformamide (80 mL). The mixture is stirred at room temperature overnight. Additional methyliodide (c=2 mol/L, 1.1 mL, 17.7 mmol) and cesium carbonate (5.0 g, 15.4 mmol) are added and the reaction is continued for 5 h. Water and ethyl acetate are added and the phases are separated. The aqueous phase is extracted twice with ethyl acetate and the combined organic phases are washed with saturated sodium chloride solution, dried over MgSO4 and concentrated. The residue is purified by reversed phase HPLC. Yield: 7.61 g. ESI mass spectrum: [M+H]+=522; Retention time HPLC: 1.20 min (HPLC method Z018_S04).

1. waitthe reaction is continued for 5 h
2. customthe phases are separated
3. extractionThe aqueous phase is extracted twice with ethyl acetate
4. washthe combined organic phases are washed with saturated sodium chloride solution
5. dry with materialdried over MgSO4
6. concentrationconcentrated
7. customThe residue is purified by reversed phase HPLC
8. custom1.20 min (HPLC method Z018_S04)