HRID606464

反应详情

EQUATION

反应方程式

HRID 606464 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-nitro-1H-1,2,4-triazole (1.00 g, 8.77 mmol), trityl chloride (4.89 g, 17.5 mmol) and diisopropylethylamine (3.05 mL, 17.5 mmol) in THF (50 mL) was stirred at room temperature for 15 hr. The mixture was concentrated under reduced pressure, and the residue was extracted with ethyl acetate and water. The organic layer was washed with saturated brine, dried over sodium sulfate, and concentrated. The residue was purified by silica gel column chromatography (15-30% ethyl acetate/hexane) to give the title compound as a white powder (2.90 g, 93%).

WORKUP

后处理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. extractionthe residue was extracted with ethyl acetate and water
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel column chromatography (15-30% ethyl acetate/hexane)