HRID1610140
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 2.2 g of 4-fluoro-1H-5-indazolecarboxylic acid methyl ester obtained in Production Example II-13-c in 20 ml dimethylformamide was added 2.12 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, 120 ml of ethyl acetate was added to the residue. 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 3.0 g of the title compound as bright yellow crystals.
WORKUP
后处理
- customAfter removing the solvent
- distillationby distillation, 120 ml of ethyl acetate
- additionwas added to the residue
- 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