反应详情

A mixture of 2-{2-[3-(pyrid-2-yl)isoxazol-5-yl]pyrrolidin-1-yl}-4-(5-methyl-1H-pyrazol-3-ylamino)pyrimidin-6-yl carboxylic acid (Method 43) (1.73 g, 4.0 mmol), methanol (300 ml) and 98% sulphuric acid (1 ml) was heated at reflux for 18 hours. The volatiles were removed by evaporation, the residue dissolved in water and the pH of the resulting solution adjusted to pH 12 with 10M sodium hydroxide. The aqueous solution was extracted with DCM and purified by chromatography on silica gel, eluting with DCM/methanol (100:0 increasing in polarity to 90:10) to give the title compound (904 mg, 51%).

1. temperaturewas heated
2. temperatureat reflux for 18 hours
3. customThe volatiles were removed by evaporation
4. dissolutionthe residue dissolved in water
5. extractionThe aqueous solution was extracted with DCM
6. custompurified by chromatography on silica gel
7. washeluting with DCM/methanol (100:0 increasing in polarity to 90:10)