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

HRID 259045

반응식

HRID 259045 반응식
[CH:1]1([CH2:9][NH2:10])[CH2:6][CH2:5][CH:4]([CH2:7][NH2:8])[CH2:3][CH2:2]1.[CH2:11]1[O:13][CH2:12]1>CO>[OH:13][CH2:12][CH2:11][NH:8][CH2:7][CH:4]1[CH2:5][CH2:6][CH:1]([CH2:9][NH2:10])[CH2:2][CH2:3]1

참가 물질

4

반응물 2

HCID 6354Ethylene Oxide2회HCID 173541,4-Cyclohexanedimethanamine

생성물 1

HCID 203734282-({[4-(Aminomethyl)cyclohexyl]methyl}amino)ethan-1-ol

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-af4c67f2f2a14770b99bf9833a8bce0d
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04035174

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