HRID2309688

反应详情

EQUATION

反应方程式

HRID 2309688 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1,2-Dihydro-8-fluoro-4-phenylimidazo[1,2-a]quinoxaline 5-oxide (3.5 g, 0.012 mol) and N-methylpiperazine (15 ml, 0.13 mol) were heated at 100° C. in isopropanol (5 ml) for 16 hrs. The solvent was removed in vacuo and the residue was dissolved in dichloromethane. The resulting solution was washed with saturated aqueous sodium hydrogen carbonate, dried over anhydrous magnesium sulphate and concentrated in vacuo to yield a dark oil which was chromatographed on silica gel in 2% methanol/chloroform to yield a red solid. The red solid was recrystallized from ethyl acetate to yield 1,2-dihydro-8-(4-methylpiperazinyl)-4-phenylimidazo[1,2-a]quinoxaline 5-oxide, (0.75 g), as deep red crystals m.p. 179°-183° C., (δ(CDCl3) 2.38 (3H,s) 2.58 (4H,m) 3.37 (4H,m) 3.95-4.24 (4H,m) 6.08 (1H,d,J=3.5Hz), 6.62 (1H,dd,J=9 and 3.5Hz), 7.38-7.5 (3H,m), 7.84 (2H,m), and 8.11 (1H,d,J=9 Hz)), represented by the structural formula: ##STR17##

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue was dissolved in dichloromethane
  3. washThe resulting solution was washed with saturated aqueous sodium hydrogen carbonate
  4. dry with materialdried over anhydrous magnesium sulphate
  5. concentrationconcentrated in vacuo
  6. customto yield a dark oil which
  7. customwas chromatographed on silica gel in 2% methanol/chloroform
  8. customto yield a red solid
  9. customThe red solid was recrystallized from ethyl acetate