反应详情

A mixture of 6-chloro-3-methyl-pyridine-2-carboxylic acid ethyl ester (650 mg, 3.26 mmol), dichloroacetic acid (5 mL) and water (0.5 mL) was refluxed for 1 h. After cooling to r.t., the mixture was neutralized with saturated NaHCO3 and extracted with CH2Cl2. The organic layer was dried over MgSO4 and concentrated in vacuo. The crude product was purified by silica gel chromatography (0-10% MeOH/CH2Cl2) to give 230 mg of the title compound as a white solid. MS: (+) m/z 182.25 (M+1).

1. temperaturewas refluxed for 1 h
2. extractionextracted with CH2Cl2
3. dry with materialThe organic layer was dried over MgSO4
4. concentrationconcentrated in vacuo
5. customThe crude product was purified by silica gel chromatography (0-10% MeOH/CH2Cl2)