Reaction #2175422

Reaction equation

EDMA

1,4-butanediol

AIBN

methacrylate

→

11-acrylamidoundecanoic acid

Solvents

water

1-propanol

Conditions

Workup

1. 1
   OtherFor the preparation of stationary phases
2. 2
   Otherpurged with nitrogen for 10 min
3. 3
   Othersealed with rubber septum
4. 4
   Otherto polymerize for 20 hours at 60° C
5. 5
   OtherThe reaction scheme for the polymerization
6. 6
   OtherAfter the polymerization of the mixture
7. 7
   Washthe monolithic column was washed with methanol for 12 hours
8. 8
   Otherto remove unreacted monomers and porogens

Procedure

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