HRID64408
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 2.5 g of methyl 5-[(2-fluorobenzyl)oxy]-6-nitronicotinate in 25 ml of THF were added 50 ml of ethanol, 25 ml of water, 218 mg of ammonium chloride, and 1.37 g of iron, followed by heating to reflux for 2 hours. After leaving to be cooled at room temperature, the reaction mixture was filtered over Celite, and to the filtrate were added a saturated aqueous sodium hydrogen carbonate solution and chloroform to carry out a layer separation operation. The organic layer was dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure to obtain 2.25 g of methyl 6-amino-5-[(2-fluorobenzyl)oxy]nicotinate.
WORKUP
后处理
- temperatureby heating
- temperatureto reflux for 2 hours
- customAfter leaving
- filtrationthe reaction mixture was filtered over Celite
- additionto the filtrate were added a saturated aqueous sodium hydrogen carbonate solution and chloroform
- customa layer separation operation
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- customthe solvent was evaporated under reduced pressure