Ethylene Oxide → 2-({[4-(Aminomethyl)cyclohexyl]methyl}amino)ethan-1-ol

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.

1. additionIn a 20 minute period, there is introduced with good agitation and beneath the liquid surface a total of 1.1 gm
2. temperatureThe reaction temperature is maintained at 45°-50° C. for an additional one-half hour
3. customThe methyl alcohol is removed by distillation at atmospheric pressure
4. customexcess 1,4-cyclohexanebis(methylamine) is readily separated from the product by fractionation under reduced pressure
5. distillationfurther purified by distillation at reduced pressure

ORDレコード

ord-af4c67f2f2a14770b99bf9833a8bce0d

出典データセット

uspto-grants-1977_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04035174