反应详情

Sodium hydride (199 mg, 4.97 mmol) was suspended in N,N-dimethylformamide (10 ml) under nitrogen atmosphere, 6-(1H-indol-5-yloxy)pyrimidin-4-ylamine (1.07 g, 4.73 mmol) synthesized in Production example 2-2 was gradually added while the reaction mixture was stirred at room temperature. After 30 minutes, the reaction mixture was cooled with an ice water bath, then phenyl N-methylcarbamate (751 mg, 4.97 mmol) synthesized in Production example 2-1 was added. The reaction mixture was heated to room temperature and stirred for 1 hour. The reaction mixture was partitioned between ethyl acetate and water. The organic layer was washed with water and brine, and was dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was purified by silica gel column chromatography (eluent; ethyl acetate) to yield the title compound (847 mg, 2.99 mmol, 63%) as white crystals.

1. additionwas gradually added while the reaction mixture
2. temperaturethe reaction mixture was cooled with an ice water bath
3. additionwas added
4. temperatureThe reaction mixture was heated to room temperature
5. stirringstirred for 1 hour
6. customThe reaction mixture was partitioned between ethyl acetate and water
7. washThe organic layer was washed with water and brine
8. dry with materialwas dried over anhydrous magnesium sulfate
9. distillationAfter the solvent was distilled off
10. customthe residue was purified by silica gel column chromatography (eluent; ethyl acetate)