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

HRID 443525

반응식

HRID 443525 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) is 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 is 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 is removed by stripping under reduced pressure to leave the product.

후처리

  1. temperaturethe mixture was then heated at 45° C.-55° C. for 3 hours
  2. customThe excess acrylonitrile is 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. customis removed
  7. customto leave the product

출처 및 근거

ORD 기록
ord-1e3cebb04cfa4adcb80a79a75f9360dd
출처 데이터셋
uspto-grants-1981_04
특허 번호
US04260760

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