反应详情

温度

50 °C

Sodium hydroxide (1.0 M in water, 1.68 mL, 1.68 mmol) was added to a solution of methyl 3-(4-(3-methyl-5-(pyrimidin-2-ylamino)phenyl)-1H-pyrazol-1-yl)cyclobutanecarboxylate (Isomer 1) (203 mg, 0.559 mmol) in methanol (4.0 mL) and water (1.0 mL). The reaction mixture was heated to 50° C. and stirred for 1 hour. The reaction mixture was cooled to ambient temperature and diluted with hydrochloric acid (1.0 M in water, 1.68 mL, 1.68 mmol) while stirring. The resulting suspension was diluted with ethyl acetate (100 mL) and brine (10 mL). The organic layer was separated, washed with brine (10 mL), dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure to afford 3-(4-(3-methyl-5-(pyrimidin-2-ylamino)phenyl)-1H-pyrazol-1-yl)cyclobutanecarboxylic acid (Isomer 1). The material was used without purification in the subsequent step. MS ESI calc'd. for C19H20N5O2 [M+H]+ 350. found 350.

1. temperatureThe reaction mixture was cooled to ambient temperature
2. stirringwhile stirring
3. customThe organic layer was separated
4. washwashed with brine (10 mL)
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure