HRID586236

反应详情

EQUATION

反应方程式

HRID 586236 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of imidazo[1,2-b][1,2,4]triazine (0.206 g, 1.715 mmol), in acetic acid (5 ml) was added sodium acetate (0.211 g, 2.27 mmol), then, dropwise over 3 min, bromine (114.8 μl, 2.23 mmol). The solution was stirred at room temperature for 30 min, then partitioned between saturated aqueous NaHCO3 (200 ml) and ethyl acetate (200 ml). The organic extracts were dried (Na2SO4), silica gel added and evaporated in vacuo. The residue was purified by chromatography (silica gel, 50% EtOAc/isohexane) to afford 0.3147 g (74%) of the title compound: 1H NMR (360 MHz, CDCl3) δ 7.25 (1H, s), 8.05 (1H, s), 8.48-8.50 (1H, m); MS (ES+) m/z 199.

WORKUP

后处理

  1. custompartitioned between saturated aqueous NaHCO3 (200 ml) and ethyl acetate (200 ml)
  2. dry with materialThe organic extracts were dried (Na2SO4), silica gel
  3. additionadded
  4. customevaporated in vacuo
  5. customThe residue was purified by chromatography (silica gel, 50% EtOAc/isohexane)