HRID1916548

反应详情

EQUATION

反应方程式

HRID 1916548 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under an argon atmosphere 6.6 g (21.0 mmol) TBAF are added to a solution of 5.8 g (20.3 mmol) 5-(4-chloro-phenyl)-2-trimethylsilanylethynyl-pyridine in 200 mL DCM at 0° C. The reaction solution is stirred for 3 h, while the reaction temperature slowly rises to RT. It is added to 50 mL water and the organic phase is extracted four times with 50 mL water, dried over MgSO4 and filtered over activated charcoal. The solvent is eliminated i.vac. and further purification is carried out by column chromatography on silica gel (PE/EtOAc 1:1).

WORKUP

后处理

  1. customslowly rises to RT
  2. extractionthe organic phase is extracted four times with 50 mL water
  3. dry with materialdried over MgSO4
  4. filtrationfiltered over activated charcoal
  5. customand further purification