反应详情

4-(4-Cyano-2-methoxycarbonyl-phenyl)-3,6-dimethyl-2-oxo-1-(3-trifluoromethyl-phenyl)-1,2,3,4-tetrahydro-pyrimidine-5-carboxylic acid ethyl ester (intermediate 9)(3.39 g, 6.76 mmol) and lithium hydroxide (194.4 mg, 8.11 mmol) are stirred in 1,4-dioxane (84 ml) and water (6.0 mL) at room temperature for 100 h. Water is added and the mixture is acidified with hydrochloric acid (4.0 mol/L) to a pH value of 3. The aqueous phase is extracted with dichloromethane three times. The combined organic phase is dried over MgSO4, concentrated and purified by reversed phase HPLC. Yield: 1.34 g. ESI mass spectrum: [M+H]+=488; Retention time HPLC: 1.08 min (HPLC method Z018_S04).

1. extractionThe aqueous phase is extracted with dichloromethane three times
2. dry with materialThe combined organic phase is dried over MgSO4
3. concentrationconcentrated
4. custompurified by reversed phase HPLC
5. custom1.08 min (HPLC method Z018_S04)