Acrylonitrile → 3,3'-[(3-Aminopropyl)azanediyl]di(propane-1,2-diol)

HRID 462323

反応式

HRID 462323 の反応式
[OH:1][CH:2]([CH2:10][OH:11])[CH2:3][NH:4][CH2:5][CH:6]([OH:9])[CH2:7][OH:8].[C:12](#[N:15])[CH:13]=[CH2:14]>>[OH:9][CH:6]([CH2:7][OH:8])[CH2:5][N:4]([CH2:3][CH:2]([OH:1])[CH2:10][OH:11])[CH2:14][CH2:13][CH2:12][NH2:15]

参加物

3

反応物 2

HCID 7855AcrylonitrileHCID 184035543,3'-Iminobispropane-1,2-diol

生成物 1

HCID 234677983,3'-[(3-Aminopropyl)azanediyl]di(propane-1,2-diol)

実験手順

Bis-(2,3-dihydroxypropyl)amine (16.5 g., 0.1 mole) and acrylonitrile (6.4 g., 0.12 mole) was mixed in an ice bath and then warmed to room temperature. After standing for 2 hours, the mixture was then heated at 45° C.-55° C. for 3 hours. The excess acrylonitrile was removed by gentle warming under reduced pressure. The residue was taken up in ethyl alcohol, mixed with sponge nickel catalyst and hydrogenated under 200 psi hydrogen using good agitation. After filtration of catalyst the solvent and excess acrylonitrile was removed by stripping under reduced pressure to leave the product as an oil.

後処理

  1. temperaturethe mixture was then heated at 45° C.-55° C. for 3 hours
  2. customThe excess acrylonitrile was removed
  3. temperatureby gentle warming under reduced pressure
  4. additionmixed with sponge nickel catalyst and hydrogenated under 200 psi hydrogen using good agitation
  5. filtrationAfter filtration of catalyst the solvent and excess acrylonitrile
  6. customwas removed

出典と根拠

ORDレコード
ord-28d32870edd2402381fa8ed4a9f87658
出典データセット
uspto-grants-1977_12
特許番号
US04065497

関連ノート

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