反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 300 mg of a compound 1H-5-indazolecarbonitrile (synthesized from 4-fluorobenzonitrile according to the procedures described in literature, Tetrahedron Lett., 33, 7499 (1992) and Synthetic commun., 27, 1199 (1997)) in 3 ml dimethylformamide was added 392 mg of N-bromosuccinimide at room temperature, and the mixture was stirred at the same temperature for one day. After removing the solvent by distillation, the residue was added with 25 ml of ethyl acetate. The mixture was sequentially washed with half-saturated aqueous sodium hydrogencarbonate solution, water and brine, dried over anhydrous magnesium sulfate and the solvent was evaporated, to give 440 mg of the title compound as pale red crystals.
WORKUP
后处理
- customAfter removing the solvent
- distillationby distillation
- additionthe residue was added with 25 ml of ethyl acetate
- washThe mixture was sequentially washed with half-saturated aqueous sodium hydrogencarbonate solution, water and brine
- dry with materialdried over anhydrous magnesium sulfate
- customthe solvent was evaporated