Réaction #2175422

ord-30bcf309d103495b8e0eac70c448f4d9

Équation de réaction

CNC(C)Cc1ccc2c(c1)OCCO2
EDMA
OCCCCO
1,4-butanediol
CC(C)(C#N)N=NC(C)(C)C#N
AIBN
C=C(C)C(=O)[O-]
methacrylate
C=CC(=O)NCCCCCCCCCCC(=O)O
11-acrylamidoundecanoic acid

Réactifs

Aucun

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutreFor the preparation of stationary phases
  2. 2
    Autrepurged with nitrogen for 10 min
  3. 3
    Autresealed with rubber septum
  4. 4
    Autreto polymerize for 20 hours at 60° C
  5. 5
    AutreThe reaction scheme for the polymerization
  6. 6
    AutreAfter the polymerization of the mixture
  7. 7
    Lavagethe monolithic column was washed with methanol for 12 hours
  8. 8
    Autreto remove unreacted monomers and porogens

Mode opératoire

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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08435410B2uspto-grants-2013_05