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Azobisisobutyronitrile → 11-(Acryloylamino)undecanoic acid

HRID 2088240
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2088240
[C:1]([O-:6])(=[O:5])[C:2](C)=[CH2:3].C[CH:8]([NH:20][CH3:21])[CH2:9][C:10]1[CH:15]=[CH:14][C:13]2OCCO[C:12]=2[CH:11]=1.C(O)CCC[OH:26].CC(N=N[C:35]([C:38]#N)(C)C)(C#N)C>O.C(O)CC>[C:21]([NH:20][CH2:8][CH2:9][CH2:10][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:3][CH2:2][C:1]([OH:6])=[O:5])(=[O:26])[CH:35]=[CH2:38]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 6547AzobisisobutyronitrileHCID 80641,4-ButanediolHCID 87595MethacrylateHCID 24257269Ethylenedioxymethylamphetamine

Produkt 1

HCID 23517111-(Acryloylamino)undecanoic acid

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel
HCID 10311-PropanolLösungsmittel

Versuchsvorschrift

For the preparation of stationary phases, the inner walls of capillaries were vinylized with 3-(trimethoxylsilyppropyl methacrylate. Subsequently, AAUA, EDMA, 1-propanol, 1,4-butanediol, water, and AIBN were mixed ultrasonically into a homogenous solution and purged with nitrogen for 10 min. A 45 cm long silanized capillary was tilled with the polymerization mixture up to a length of 35 cm, sealed with rubber septum, and then placed in a gas chromatography (GC) oven to polymerize for 20 hours at 60° C. The reaction scheme for the polymerization is shown in Scheme 1. Each column of the experimental design was made in duplicate. After the polymerization of the mixture, the monolithic column was washed with methanol for 12 hours using a HPLC pump to remove unreacted monomers and porogens. An on-column detection window was made next to the polymer bed using a thermal wire stripper. Finally, the column was cut to 45 cm with an effective length of 30 cm.

Aufarbeitung

  1. customFor the preparation of stationary phases
  2. custompurged with nitrogen for 10 min
  3. customsealed with rubber septum
  4. customto polymerize for 20 hours at 60° C
  5. customThe reaction scheme for the polymerization
  6. customAfter the polymerization of the mixture
  7. washthe monolithic column was washed with methanol for 12 hours
  8. customto remove unreacted monomers and porogens

Quellen und Nachweise

ORD-Eintrag
ord-30bcf309d103495b8e0eac70c448f4d9
Quelldatensatz
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08435410B2

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