HRID2237637

反应详情

EQUATION

反应方程式

HRID 2237637 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-bromoacetylpyridine hydrobromide (5 g, 17.8 mmol) in 20 mL of water was added sodium azide (1.16 g, 17.8 mmol) and the contents stirred at room temperature for 2 h. The reaction mixture was treated with saturated aqueous NaHCO3 until neutrality, extracted with ethyl acetate (3×30 mL) and the combined organic phases were dried over MgSO4. After solvent removal the crude residue was silica gel column chromatographed (dichloromethane/ethanol/98/2). 3-Azidoacetyl-pyridine was obtained as yellow solid (2.17 g, 71%).

WORKUP

后处理

  1. extractionextracted with ethyl acetate (3×30 mL)
  2. dry with materialthe combined organic phases were dried over MgSO4
  3. customAfter solvent removal the crude residue
  4. customchromatographed (dichloromethane/ethanol/98/2)