HRID503128

反应详情

EQUATION

反应方程式

HRID 503128 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 5.0 g of 6-nitro-1H-indazole in 50 ml dimethylformamide was added 5.73 g of N-bromosuccinimide at room temperature, and the mixture was stirred at the same temperature for 1 hour. After removing the solvent by distillation, the residue was added with 250 ml of ethyl acetate. The mixture was sequentially washed with half-saturated aqueous sodium hydrogencarbonate solution, water and brine, and dried over anhydrous magnesium sulfate. After filtrating the organic layer through a silica gel pat, the solvent was evaporated and the resulting crystals were suspended in toluene, to give 6.59 g of the title compound as light brown crystals.

WORKUP

后处理

  1. customAfter removing the solvent
  2. distillationby distillation
  3. additionthe residue was added with 250 ml of ethyl acetate
  4. washThe mixture was sequentially washed with half-saturated aqueous sodium hydrogencarbonate solution, water and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationAfter filtrating the organic layer through a silica gel pat
  7. customthe solvent was evaporated