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

HRID 1439779

반응식

HRID 1439779 반응식
[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]

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5c6164dd392749ceae5643ee7bebf89a
출처 데이터셋
uspto-grants-1977_11
특허 번호
US04060639

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