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

HRID 259045
ノート
印刷プレビュー

反応式

HRID 259045 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6354Ethylene Oxide2 回HCID 173541,4-Cyclohexanedimethanamine

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

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

反応ノート

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