反应详情

To a solution of 2-chloro-4-trifluoromethylpyrimidine-5-carbonyl chloride (0.50 g, 2.0 mmol) in THF at -78° C. under N2 was added MeMgBr (0.75 ml, 2.3 mmol). The reaction was stirred 0.75 h, quenched with H2O (1 ml) and diluted with EtOAc (30 ml). The organic layer was washed with H2O, brine and then dried over MgSO4. The residue was chromatographed (SiO2, hexanes/EtOAc, 2:1) to provide the 5-acetyl-2-chloro-4-trifluoromethylpyrimidine (0.20 g) in 43% yield. The title compound was then prepared as described for ethyl 2-[N-(1'-aminocitraconamide)]-4-trifluoromethylpyrimidine-5-carboxylate of Example 20, resulting in a 29% yield (0.08 g); m.p. 61°-62° C.

1. customquenched with H2O (1 ml)
2. additiondiluted with EtOAc (30 ml)
3. washThe organic layer was washed with H2O, brine
4. dry with materialdried over MgSO4
5. customThe residue was chromatographed (SiO2, hexanes/EtOAc, 2:1)