HRID1931739
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 180 °C
PROCEDURE
实验过程
A mixture of 2-fluoro-4-methanesulfonyl-phenol (Intermediate 1; 101 mg, 0.53 mmol), 4-chloro-1-[4-(3-isopropyl-[1,2,4]oxadiazol-5-yl)-cis-cyclohexyl]-1H-pyrazolo[3,4-d]pyrimidine (Intermediate 25; 185 mg, 0.53 mmol) and potassium carbonate (48 mg, 0.53 mmol) in anhydrous DMF (5 mL) was heated in a microwave at 180° C. for 10 min. The mixture was filtered. The filtrate was concentrated and purified using a Supelco 23 g column, eluting with 0-3% methanol/dichloromethane to give 4-(2-fluoro-4-methanesulfonyl-phenoxy)-1-[4-(3-isopropyl-[1,2,4]oxadiazol-5-yl)-cis-cyclohexyl]-1H-pyrazolo[3,4-d]pyrimidine (148 mg, 56%).
WORKUP
后处理
- filtrationThe mixture was filtered
- concentrationThe filtrate was concentrated
- custompurified
- washeluting with 0-3% methanol/dichloromethane