反应详情

温度

140 °C

A mixture of ethyl 4-(4-chloro-5H-pyrrolo[3,2-d]pyrimidin-6-yl)benzoate hydrochloride (1.297 g), 3-methyl-4-[(6-methylpyridin-3-yl)oxy]aniline (1.00 g), diisopropylethylamine (0.834 g) and 1-methyl-2-pyrrolidinone (12.5 mL) was stirred at 140° C. for 3 hrs, poured into water (100 mL)-ethyl acetate (150 mL) and the precipitated solid was collected by filtration. The solid washed with ethyl acetate and dried under reduced pressure at 60° C. The obtained solid was suspended in methanol (40 mL), and 1N aqueous sodium hydroxide solution (20 mL) was added. After stirring at room temperature for 12 hrs, the solvent was evaporated under reduced pressure, and the residue was adjusted to pH 2 with 1N hydrochloric acid. The precipitated solid was collected by filtration, washed with water and dried under reduced pressure at 60° C. to give the title compound (1.08 g).

1. filtrationthe precipitated solid was collected by filtration
2. washThe solid washed with ethyl acetate
3. customdried under reduced pressure at 60° C
4. addition1N aqueous sodium hydroxide solution (20 mL) was added
5. stirringAfter stirring at room temperature for 12 hrs
6. customthe solvent was evaporated under reduced pressure
7. filtrationThe precipitated solid was collected by filtration
8. washwashed with water
9. customdried under reduced pressure at 60° C.