反应详情

温度

160 °C

A solution of 6-chloro-N-(4-hydroxy-2-methylphenyl)pyrimidine-4-carboxamide, Intermediate 7 (50.0 mg; 0.20 mmol) in ethanol (3 mL) was treated with N-ethyldiisopropylamine (69 μl; 0.4 mmol) and o-toluidine (Fluka, 21.5 μl; 0.20 mmol). The reaction mixture was heated at 160° C. for 3 hours under microwave irradiation. The solvents were removed in vacuo, EtOAc was added and the organic phase was washed with a citric acid solution, dried over magnesium sulfate then evaporated in vacuo. The crude product was purified by column chromatography (silica), eluting with cyclohexane containing an increasing amount of EtOAc. The title compound was obtained as a yellow solid.

1. customThe solvents were removed in vacuo, EtOAc
2. additionwas added
3. washthe organic phase was washed with a citric acid solution
4. dry with materialdried over magnesium sulfate
5. customthen evaporated in vacuo
6. customThe crude product was purified by column chromatography (silica)
7. washeluting with cyclohexane containing an increasing amount of EtOAc