反应详情

温度

180 °C

A mixture of 4-(1,2,4)-triazol-1-yl-phenol (Lancaster; 14 mg, 0.09 mmol), 4-(4-chloro-pyrazolo[3,4-d]pyrimidin-1-yl)-piperidine-1-carboxylic acid tert-butyl ester (Intermediate 19; 29.5 mg, 0.09 mmol) and potassium carbonate (14.4 mg, 0.10 mmol) in anhydrous DMF (1 mL) was heated in a microwave at 180° C. for 10 min. The mixture was cooled and filtered. The solid was washed with dichloromethane. The filtrate was concentrated and purified using a 4 g silica gel column, eluting with 0-5% methanol/dichloromethane to give 4-[4-(4-[1,2,4]triazol-1-yl-phenoxy)-pyrazolo[3,4-d]pyrimidin-1-yl]-piperidine-1-carboxylic acid tert-butyl ester (17 mg, 42%).

1. temperatureThe mixture was cooled
2. filtrationfiltered
3. washThe solid was washed with dichloromethane
4. concentrationThe filtrate was concentrated
5. custompurified
6. washeluting with 0-5% methanol/dichloromethane