HRID1931739

反应详情

EQUATION

反应方程式

HRID 1931739 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationThe mixture was filtered
  2. concentrationThe filtrate was concentrated
  3. custompurified
  4. washeluting with 0-3% methanol/dichloromethane