反应详情

Methyl 4-amino-3-chloro-5-fluoro-6-(4-chlorophenyl)pyridine-2-carboxylate (0.545 g, 1.73 mmol) was suspended in decanol (20 mL) and titanium methoxide (0.029 g, 1.73 mmol) was added and the mixture heated under reflux for five hours. The reaction mixture was concentrated and the residue dissolved in ethyl acetate (100 mL) and washed with water (100 mL) and saturated sodium bicarbonate solution (100 mL). The organic phase was dried (MgSO4) and concentrated to give decyl 4-amino-3-chloro-5-fluoro-6-(4-chlorophenyl)pyridine-2-carboxylate (0.67 g, 1.5 mmol), mp 62-63° C.

1. temperaturethe mixture heated
2. temperatureunder reflux for five hours
3. concentrationThe reaction mixture was concentrated
4. dissolutionthe residue dissolved in ethyl acetate (100 mL)
5. washwashed with water (100 mL) and saturated sodium bicarbonate solution (100 mL)
6. dry with materialThe organic phase was dried (MgSO4)
7. concentrationconcentrated