HRID456042

反应详情

EQUATION

反应方程式

HRID 456042 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 6-chloroimidazo[1,2-b]pyridazine (5 g, 32.6 mmol) in acetonitrile (300 ml) was added 1-bromopyrrolidine-2,5-dione (6.37 g, 35.8 mmol) and trifluoroacetic acid (0.75 mL). The resulting solution was allowed to stir at room temperature overnight. The solvent was removed under reduced pressure and the residue was dissolved in EtOAc, washed with NaHCO3 solution, water and brine, dried over Na2SO4 and concentrated in vacuo to afford 7.2 g title compound in 92% yield as a light yellow solid. 1H-NMR (400 MHz, CDCl3) δ ppm 7.91 (d, 1H), 7.79 (s, 1H), 7.12 (d, 1H). LCMS (method A): [MH]+=232/234, tR=4.48 min.

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. dissolutionthe residue was dissolved in EtOAc
  3. washwashed with NaHCO3 solution, water and brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo