HRID1172566
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
2-Furan-2-yl-5-methanesulfonyl-[1,2,4]triazolo[1,5-a][1,3,5]triazin-7-ylamine (0.7 mmol, 1 eq.; see J. Chem. Soc. Perkin Trans. 1, 801 (1995)) and 2,5-diaza-bicyclo[2.2.1]heptane (5 eq.) were suspended in 10 mL of CH3CN. The mixture was stirred under reflux for 2 hours. It was then cooled to room temperature and concentrated under reduced pressure. The residue was taken up in CH2Cl2 and washed with water, brine, dried with Na2SO4, and concentrated under reduced pressure. The resulting crude product was purified by column chromatography (95% CH2Cl2, 4% MEOH, 1% Et3N) to afford 5-(2,5-diaza-bicyclo[2.2.1]hept-2-yl)-2-furan-2-yl-[1,2,4]triazolo[1,5-a][1,3,5]triazin-7-ylamine.
WORKUP
后处理
- temperatureunder reflux for 2 hours
- concentrationconcentrated under reduced pressure
- washwashed with water, brine
- dry with materialdried with Na2SO4
- concentrationconcentrated under reduced pressure
- customThe resulting crude product was purified by column chromatography (95% CH2Cl2, 4% MEOH, 1% Et3N)