HRID606464
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- concentrationThe mixture was concentrated under reduced pressure
- extractionthe residue was extracted with ethyl acetate and water
- washThe organic layer was washed with saturated brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated
- customThe residue was purified by silica gel column chromatography (15-30% ethyl acetate/hexane)