HRID1481955

反应详情

EQUATION

反应方程式

HRID 1481955 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-[2-Azido-2-(2-hydroxy-ethoxy)-ethoxy]-benzoic acid ethyl ester (1.34 g, 4.55 mmol) was stirred with 4 M aqueous sodium hydroxide (11.4 ml, 45.5 mmol) and ethanol (11.4 ml) at room temperature. After 3 hrs, all the solvents were removed under reduced pressure and the residue was dissolved in 50 ml water. The solution was acidified with 1 N HCl to pH 2 and then extracted with DCM (3×50 ml). All the DCM extracts were combined, dried over MgSO4 and evaporated under reduced pressure. The title compound was obtained as a colourless solid (1.2 g, 98.7%). ES-MS, m/z 265.85 (M−1).

WORKUP

后处理

  1. customall the solvents were removed under reduced pressure
  2. dissolutionthe residue was dissolved in 50 ml water
  3. extractionextracted with DCM (3×50 ml)
  4. dry with materialdried over MgSO4
  5. customevaporated under reduced pressure