HRID588148

反应详情

EQUATION

反应方程式

HRID 588148 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

4,6-dichloro-3-methoxy-1-trityl-1H-pyrazolo[4,3-c]pyridine (37B, 75 mg, 0.163 mmol), 2-methylpyridine-4-boronic acid pinacol ester (39.3 mg, 0.179 mmol), and Xphos Precatalyst 2nd generation (10.25 mg, 0.013 mmol) were taken up in THF (1.1 ml). The mixture was evacuated and back-filled with N2 gas (3×). Potassium phosphate tribasic (104 mg, 0.489 mmol) in Water (543 μl) (degassed) was then added to the reaction mixture. The reaction was allowed to stir at 60° C., for 1 hour. The reaction was then filtered through celite and loaded onto silica gel. The reaction mixture was purified by MPLC 0-50% EtOAc/DCM to give 6-chloro-3-methoxy-4-(2-methylpyridin-4-yl)-1-trityl-1H-pyrazolo[4,3-c]pyridine (49B). MS: [M+H]+ m/z 517.

WORKUP

后处理

  1. customThe mixture was evacuated
  2. additionback-filled with N2 gas (3×)
  3. filtrationThe reaction was then filtered through celite and
  4. customThe reaction mixture was purified by MPLC 0-50% EtOAc/DCM