HRID2230077

反应详情

EQUATION

反应方程式

HRID 2230077 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The reaction mixture of nalidixic acid (232 mg, 1.0 mmol), metronidazole (171 mg, 1.0 mmol), EDCI (230 mg, 1.2 mmol), DMAP (20 mg, 0.2 mmol) and THF (5 ml) was stirred at room temperature for 24 h. THF was then removed under reduced pressure. The residue was dissolved in dichloromethane (50 ml). The organic layer was washed with H2O, 5% Na2CO3, H2O, and brine, and then dried over MgSO4. The solvent was removed under vacuum. The resulting solid was recrystallized from C2H5OH and ethyl acetate to give 56 mg 2-methyl-5-nitro-1H-imidazole-1-ethyl 1-ethyl-1,4-dihydro-7-methyl-4-oxo-1,8-naphthyridine-3-carboxylate. m.p.: 122-124° C.

WORKUP

后处理

  1. customTHF was then removed under reduced pressure
  2. dissolutionThe residue was dissolved in dichloromethane (50 ml)
  3. washThe organic layer was washed with H2O, 5% Na2CO3, H2O, and brine
  4. dry with materialdried over MgSO4
  5. customThe solvent was removed under vacuum
  6. customThe resulting solid was recrystallized from C2H5OH and ethyl acetate