反应详情

温度

50 °C

A mixture of {3,5-dichloro-4-[7-fluoro-4-(6-hydroxymethylpyrimidin-4-ylamino)-thiazolo[5,4-c]pyridin-2-yl]phenyl}-carbamic acid tert-butyl ester (102 mg, 0.19 mmol) in HCl (4 N in dioxane, 3 mL) under a nitrogen atmosphere was heated at 50° C. for 5 hours. After cooling to room temperature, the precipitate was collected by filtration and then purified by column chromatography on silica gel eluting with 0-5% MeOH in EtOAc. To the resultant solid obtained was added DCM (1 mL) followed by HCl (4 N in dioxane, 1 mL) and the resulting mixture was stirred at room temperature for 1 hour and then concentrated under reduced pressure to afford the title compound as an off white solid (50 mg, 91% yield). 1H NMR (300 MHz, DMSO-d6): δ 11.75 (br s, 1H), 8.89 (s, 1H), 8.57 (d, J=2.1 Hz, 1H), 7.70 (s, 1H), 6.78 (s, 2H), 4.61 (s, 2H). LCMS (Method C): RT=3.11 min, m/z: 437 [M+H+].

1. temperatureAfter cooling to room temperature
2. filtrationthe precipitate was collected by filtration
3. custompurified by column chromatography on silica gel eluting with 0-5% MeOH in EtOAc
4. customTo the resultant solid obtained
5. concentrationconcentrated under reduced pressure