HRID2417705
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
A solution of 12 g of ammonium acetate in 45 ml of water was added to a solution of 15 g of 4-(2,4-difluorobenzoyl)-1-formylpiperidine and 6 g of hydroxylamine hydrochloride in 35 ml of ethanol. The mixture was heated for 18 at 90°, with stirring. The solution was evaporated in vacuum until precipitation occurred. Water (500 ml) was added. The mixture was filtered, washed with 300 ml of water and dried in vacuum over phosphorous pentoxide to yield 12 g (75.5%) of product. Recrystallization from ethanol and water yielded the analytical sample, mp, 185°.
WORKUP
后处理
- temperatureThe mixture was heated for 18 at 90°
- customThe solution was evaporated in vacuum until precipitation
- additionWater (500 ml) was added
- filtrationThe mixture was filtered
- washwashed with 300 ml of water
- dry with materialdried in vacuum over phosphorous pentoxide