HRID2072730

反应详情

EQUATION

反应方程式

HRID 2072730 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 3-amino-5-(1-(3-benzoylphenyl)ethyl)-1,2,4-oxadiazole (1.20 g, 4.09 mmol) in toluene (10 ml) were added ethyleneglycol (0.80 g, 12.9 mmol) and p-toluenesulfonic acid monohydrate (0.025 g, 0.15 mmol). After reflux for 10 h, the mixture was cooled at room temperature and extracted with toluene. The extracts were washed with aqueous sodium hydrogen carbonate and then water, dried with anhydrous sodium sulfate, and evaporated under reduced pressure to a residue, which was chromatographed to afford 3-amino-5-(1-(3-(2-phenyl-1,3-dioxolan-2-yl)phenyl)ethyl)-1,2,4-oxadiazole (1.06 g, 77% yield) as crystalline material: mp 112.0°-113.5° C.

WORKUP

后处理

  1. temperatureAfter reflux for 10 h
  2. extractionextracted with toluene
  3. washThe extracts were washed with aqueous sodium hydrogen carbonate
  4. dry with materialwater, dried with anhydrous sodium sulfate
  5. customevaporated under reduced pressure to a residue, which
  6. customwas chromatographed