HRID1627922

反应详情

EQUATION

反应方程式

HRID 1627922 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

7-bromo-2.3-dihydropyrano[4.3.2-de]quinoline (0.170 g; 0.680 mmol), bis(pinacolato)diboron (0.207 g; 0.816 mmol), anhydrous potassium acetate (0.133 g; 1.36 mmol) and bis(tricyclohexylphosphine)palladium(0) (0.045 g; 0.068 mmol) in anhydrous 1.4-dioxane (3.1 mL) were mixed in a tube, purged with argon and sealed. After heating at 95° C. for 16 h, the mixture was cooled at room temperature, concentrated under reduced pressure and store at 3° C. for 21 h. The brown residue was dissolved in acetonitrile, filtered, and the dark brown solution was concentrated under reduced pressure. Purification by preparative HPLC (HPLC method 1) furnished 0.044 g (25%) of the title compound as an amorphous solid.

WORKUP

后处理

  1. custompurged with argon
  2. customsealed
  3. temperaturethe mixture was cooled at room temperature
  4. concentrationconcentrated under reduced pressure and store at 3° C. for 21 h
  5. dissolutionThe brown residue was dissolved in acetonitrile
  6. filtrationfiltered
  7. concentrationthe dark brown solution was concentrated under reduced pressure
  8. customPurification by preparative HPLC (HPLC method 1)