HRID632798

反应详情

EQUATION

反应方程式

HRID 632798 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 1-methyl-3-(1-methyl-1H-pyrazol-3-yl)imidazolidin-2-one (161 mg) in acetic anhydride (2.1 mL) was added fuming nitric acid (0.074 mL) under ice-cooling, and the mixture was stirred for 1.5 hr under ice-cooling. The reaction mixture was poured into ice water, and the mixture was neutralized with saturated aqueous sodium hydrogen carbonate solution, and extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (methanol/ethyl acetate) to give the title compound (101 mg).

WORKUP

后处理

  1. temperaturecooling
  2. temperaturecooling
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (methanol/ethyl acetate)