HRID2353396

反应详情

EQUATION

反应方程式

HRID 2353396 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 4,7-dibromo-5-fluoro-3-[6-(methyloxy)-3-pyridinyl]-1H-indazole and 6-bromo-5-fluoro-3-[6-(methyloxy)-3-pyridinyl]-1H-indazole (2:1) (Intermediate 9, 20 mg), N-ethyl-4-methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzamide (Intermediate 10, 32 mg), 1M aqueous sodium bicarbonate (1 ml) and tetrakis(triphenylphosphine)palladium (6 mg) in isopropanol was heated in a sealed vessel by microwave at 150° C. for 15 min. The reaction mixture was partitioned between chloroform and water and the organic layer was separated using a hydrophobic filter tube. The organic layer was concentrated under vacuum and the residue was purified by reverse phase preparative HPLC to give the title compound (3 mg).

WORKUP

后处理

  1. customThe reaction mixture was partitioned between chloroform and water
  2. customthe organic layer was separated
  3. concentrationThe organic layer was concentrated under vacuum
  4. customthe residue was purified by reverse phase preparative HPLC