HRID1384542
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
CONDITIONS
反应条件
- 温度
- 5 °C
PROCEDURE
实验过程
Thionyl chloride (0.75 ml, 10 mmol) was added to a solution of 4-(2-hydroxyethoxy)pyridine (0.9 g, 6.5 mmol), (J. Chem. Soc. Perkin II, 1987, 1867), in trichloromethane (20 ml) at 5° C. The mixture was stirred for 1 hour at 5° C., allowed to warm to ambient temperature and stirred for a further 2 hours. The volatiles were removed by evaporation and by azeotroping with toluene to give 4-(2-chloroethoxy)pyridine hydrochloride (1.3 g, 100%). 1H NMR Spectrum: (DMSOd6) 4.03(t, 2H); 4.62(t, 2H); 7.58(d, 2H); 8.77(d, 2H) MS-ESI: 158 [MH]+
WORKUP
后处理
- temperatureto warm to ambient temperature
- stirringstirred for a further 2 hours
- customThe volatiles were removed by evaporation
- customby azeotroping with toluene