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 14.2 gm. (0.1 mole) of 1,4-cyclohexanebis(methylamine) in 150 ml. anhydrous methyl alcohol and under an atmosphere of nitrogen is warmed to 45°-50° C. In a 20 minute period, there is introduced with good agitation and beneath the liquid surface a total of 1.1 gm. (0.025 mole) of ethylene oxide in gaseous form. The reaction temperature is maintained at 45°-50° C. for an additional one-half hour after stopping the addition of ethylene oxide. The methyl alcohol is removed by distillation at atmospheric pressure; excess 1,4-cyclohexanebis(methylamine) is readily separated from the product by fractionation under reduced pressure. Only monoethoxylated compound remains and can be used as such or further purified by distillation at reduced pressure.
WORKUP
后处理
- additionIn a 20 minute period, there is introduced with good agitation and beneath the liquid surface a total of 1.1 gm
- temperatureThe reaction temperature is maintained at 45°-50° C. for an additional one-half hour
- customThe methyl alcohol is removed by distillation at atmospheric pressure
- customexcess 1,4-cyclohexanebis(methylamine) is readily separated from the product by fractionation under reduced pressure
- distillationfurther purified by distillation at reduced pressure