反应详情

温度

40 °C

To a solution of methyl 2-[(2-methoxyethoxy)methoxy]-3-(5-methoxypyridin-2-ylamino)benzoate 1.0 g (2.8 mmol) of step 3 in methanol 20 mL was added 6NHCl 2 mL, followed by stirring at 40° C. for 30 min. The reaction mixture was cooled to room temperature, concentrated in a vacuum, diluted with ethylacetate, washed with distilled water, and a saturated NaCl solution. After drying over magnesium sulfate and concentration in a vacuum, purification by column chromatography (developing solvent: ethylacetate/hexane=1/2) afforded 0.70 g of the title compound (yield 90%).

1. temperatureThe reaction mixture was cooled to room temperature
2. concentrationconcentrated in a vacuum
3. additiondiluted with ethylacetate
4. washwashed with distilled water
5. dry with materialAfter drying over magnesium sulfate and concentration in a vacuum, purification by column chromatography (developing solvent: ethylacetate/hexane=1/2)