反应详情

50-72% Oily sodium hydride (265 mg) was added to a solution of 4-((6-(2-ethoxyethoxy)-1H-indol-5-yl)oxy)pyridin-2-amine described in Production Example 24-7 (1.92 g, 6.13 mmol) in N,N-dimethylformamide (20 mL) under nitrogen atmosphere at 0° C. The reaction liquid was stirred at the same temperature for 10 minutes. Phenyl methylcarbamate described in Production Example 1-7 (1.20 g, 7.97 mmol) was added to the reaction liquid, and then the mixture was warmed to mom temperature and stirred for 1 hour. Water and ethyl acetate were added to the reaction liquid. The organic layer was washed serially with water and a saturated saline solution and then dried over anhydrous sodium sulfate. The drying agent was separated by filtration and then the filtrate was concentrated under vacuum. The residue was purified with NH silica gel column chromatography (the solution: n-heptane:ethyl acetate=9:1-0:1) to obtain the title compound (1.97 g, 87%).

1. customThe reaction liquid
2. additionwas added to the reaction liquid
3. temperaturethe mixture was warmed to mom temperature
4. stirringstirred for 1 hour
5. washThe organic layer was washed serially with water
6. dry with materiala saturated saline solution and then dried over anhydrous sodium sulfate
7. customThe drying agent was separated by filtration
8. concentrationthe filtrate was concentrated under vacuum
9. customThe residue was purified with NH silica gel column chromatography (the solution