反应详情

To a cold (0° C.) suspension of NaH (400 mg, 9.96 mmol, 60% in oil) in THF (8 mL) was slowly added ethylacetoacetate (1.45 mL, 11.5 mmol). The solution was allowed to stir at rt for 10 min then concentrated in vacuo. The residue was rapidly put under N2. A solution of 2,4-dichloro-6-[(2,2,2-trifluoroethoxy)methyl]pyrimidine (2.0 g, 7.66 mmol) in toluene (38 mL) was added to the residue. The reaction mixture was stirred under reflux for 16 h. Ammonium chloride (aq, 1 mL) was added and stirred vigorously for 10 min. Silica was added and the mixture was concentrated. The residue was purified on a silica gel cartridge eluting with 0% to 40% EtOAc/heptanes to give ethyl the title compound, 600 mg (28%).

1. concentrationthen concentrated in vacuo
2. stirringThe reaction mixture was stirred
3. temperatureunder reflux for 16 h
4. stirringstirred vigorously for 10 min
5. additionSilica was added
6. concentrationthe mixture was concentrated
7. customThe residue was purified on a silica gel cartridge
8. washeluting with 0% to 40% EtOAc/heptanes