HRID2109794

反应详情

EQUATION

反应方程式

HRID 2109794 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a stirred mixture of bis(pinacolato)diboron (6.4 g, 25 mmol), potassium acetate (6.8 g, 69 mmol), dichloro[1,1′bis(diphenylphoshino)ferrocene]palladium(II)dichloromethane adduct (0.50 g, 0.69 mmol), and 6-bromo-4-chlorocinnoline (5.60 g, 23 mmol), was added DMF (50.00 mL, 646 mmol) and the overall mixture was heated at 80° C. overnight. After cooling and checking by LC-MS, the overall mixture was concentrated with silica and purified with ISCO (40 g, hexanes/EA, 1:0 to 1:1) to provide the title compound 6-bromocinnoline (1.48, 31%) as a yellow solid. LCMS (API-ES) m/z (%): 210.0 (100%, M++H).

WORKUP

后处理

  1. temperatureAfter cooling
  2. concentrationthe overall mixture was concentrated with silica
  3. custompurified with ISCO (40 g, hexanes/EA, 1:0 to 1:1)