反应详情

To a stirred suspension of 4-{5-(cyclopropylcarbonyl)-6-methyl-2-oxo-1-[3-(trifluoromethyl)phenyl]-1,2,3,4-tetrahydropyrimidin-4-yl}benzonitrile (Example 22) (150 mg, 0.35 mmol) and potassium carbonate (98 mg, 0.71 mmol) in dimethylformamide (3 ml) is added methyl 2-(chloromethyl)-1,3-oxazole-4-carboxylate (93 mg, 0.53 mmol). The reaction mixture is stirred at room temperature overnight, then an additional equivalent of potassium carbonate (0.35 mmol) and methyl 2-(chloromethyl)-1,3-oxazole-4-carboxylate (0.35 mmol) are added, and the solution is stirred an additional 72 hours. The reaction mixture is quenched with water (20 ml) and extracted with ethyl acetate (3×50 ml). The combined organic phases are washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated. The residue is purified by HPLC (RP18 column; eluent: acetonitrile/water 30:70→90:10).

1. stirringthe solution is stirred an additional 72 hours
2. customThe reaction mixture is quenched with water (20 ml)
3. extractionextracted with ethyl acetate (3×50 ml)
4. washThe combined organic phases are washed with brine
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue is purified by HPLC (RP18 column; eluent: acetonitrile/water 30:70→90:10)