HRID454868

反应详情

EQUATION

反应方程式

HRID 454868 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 6-chloro-1-(4-fluoro-2-methylphenyl)phthalazine (0.197 g, 0.72 mmol), palladium(II) acetate (0.011 g, 0.049 mmol), 1,1′-bis(isopropylphosphino)ferrocene (0.022 g, 0.053 mmol) and 3-fluorothiophenol (0.080 ml, 0.95 mmol) in 2 mL of Et3N was sealed in a glass tube purged with argon and heated at 100° C. in an oil bath for 17 h. The reaction mixture was cooled to RT and diluted with MeOH. The solution was evaporated onto silica gel and purified by flash chromatography (ISCO 80 g column, eluting with 15-45% EtOAc in hexanes) to give the title compound as a white amorphous solid. MS (ESI, pos. ion) m/z: M+1=365.1

WORKUP

后处理

  1. customwas sealed in a glass tube
  2. custompurged with argon
  3. temperatureThe reaction mixture was cooled to RT
  4. additiondiluted with MeOH
  5. customThe solution was evaporated onto silica gel
  6. custompurified by flash chromatography (ISCO 80 g column, eluting with 15-45% EtOAc in hexanes)