HRID2423100

反应详情

EQUATION

反应方程式

HRID 2423100 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of 6-bromo-1-(3-fluoro-4-hydroxyphenyl)-1H-indazol-4-ol (360 mg, 1.11 mmol) (E5) in dimethoxyethane (10 mL) was added dichlorobis(tris-o-tolylphosphine)palladium (44 mg, 0.056 mmol) and tributylvinyltin (0.65 mL, 2.22 mmol). The reaction mixture was heated at 90° C. under argon overnight. After cooling to room temperature, the mixture was filtered through a pad of celite. The filtrate was concentrated and the crude product purified by silica gel chromatography eluting with 5-100% ethyl acetate in hexane. The product was further purified by MDAP to yield the title compound (E6) (101 mg).

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. filtrationthe mixture was filtered through a pad of celite
  3. concentrationThe filtrate was concentrated
  4. customthe crude product purified by silica gel chromatography
  5. washeluting with 5-100% ethyl acetate in hexane
  6. customThe product was further purified by MDAP