HRID2216891

反应详情

EQUATION

反应方程式

HRID 2216891 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The crude 4-tributylstannyl-1-trityl-1H-imidazole (1.37 g) in toluene (10 mL) was treated sequentially with 2-bromopyridine (0.33 mL, 3.43 mmol) and Pd(PPh3)4 (0.26 g, 0.23 mmol). The reaction mixture was heated at reflux under an argon atmosphere for 4 hours. After cooling, the reaction mixture was concentrated in vacuo. The residue was dissolved in chloroform (50 mL) and sequentially washed with aqueous saturated potassium fluoride (75 mL), water (75 mL) and brine (100 mL). The organic phase was dried over anhydrous sodium sulfate, filtered and concentrated in-vacuo to afford 0.69 g of crude 4-(2-pyridyl)-1-trityl-1H-imidazole.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux under an argon atmosphere for 4 hours
  3. temperatureAfter cooling
  4. concentrationthe reaction mixture was concentrated in vacuo
  5. dissolutionThe residue was dissolved in chloroform (50 mL)
  6. washsequentially washed with aqueous saturated potassium fluoride (75 mL), water (75 mL) and brine (100 mL)
  7. dry with materialThe organic phase was dried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in-vacuo