HRID1655549
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
2.5 g (22.9 mmol) of p-aminophenol, 3.09 g (22.9 mmol) of 1,2-dichloro-1,1-difluoroethane, 5.48 g (39.6 mmol) of K2CO3 and 40 ml of dry acetonitrile were stirred together at room temperature for 5 days. The mixture was poured into water and extracted two times into ether. The combined ether extracts were washed with water, dried over MgSO4 and filtered: HCl gas was bubbled into the ether solution causing the above-named aniline to precipitate as the hydrochloride salt, which was collected by filtration and recrystallized twice from CH3CN to give 0.9 g (16 percent of theoretical d 245°-250° C.) of a white solid.
WORKUP
后处理
- extractionextracted two times into ether
- washThe combined ether extracts were washed with water
- dry with materialdried over MgSO4
- filtrationfiltered
- customHCl gas was bubbled into the ether solution
- customto precipitate as the hydrochloride salt, which
- filtrationwas collected by filtration
- customrecrystallized twice from CH3CN
- customto give 0.9 g (16 percent of theoretical d 245°-250° C.) of a white solid