HRID45603

反应详情

EQUATION

反应方程式

HRID 45603 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

1-(4′-{3-Methyl-4-[6-bromo-pyridin-2-ylamino]-isoxazol-5-yl}-biphenyl-4-yl)-cyclopropanecarboxylic acid ethyl ester (0.050 g, 0.09 mmol), o-tolylboronic acid (0.016 g, 0.12 mmol), sodium bicarbonate (0.040 g, 0.48 mmol), and bis(diphenylphosphino)ferrocene)-dichloropalladium(II) (0.007 g, 0.009 mmol) were combined in 3:1 DME:H2O (2 mL) and warmed with stirring to 70° C. After 3 hrs, the mixture was cooled to room temperature diluted with EtOAc (30 mL) and extracted with H2O (2×10 mL). The organic layer was dried over MgSO4, filtered and concentrated, and the crude residue was purified on reverse-phase preparative HPLC to afford the title compound.

WORKUP

后处理

  1. temperaturethe mixture was cooled to room temperature
  2. extractionextracted with H2O (2×10 mL)
  3. dry with materialThe organic layer was dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customthe crude residue was purified on reverse-phase preparative HPLC