HRID1172566

反应详情

EQUATION

反应方程式

HRID 1172566 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureunder reflux for 2 hours
  2. concentrationconcentrated under reduced pressure
  3. washwashed with water, brine
  4. dry with materialdried with Na2SO4
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting crude product was purified by column chromatography (95% CH2Cl2, 4% MEOH, 1% Et3N)