反应详情

Dimethylacrylamide (3.35 gm, 33.8 mmole), 6-acetoxyhexylacrylamide (0.409 gm, 1.92 mmole) and N,N'-bisacryloyl-2,2-di-(2-aminoethoxy)propane (0.627 gm, 2.32 mmole) were dissolved in 8 mL of DMF and N2 gas was bubbled through the solution for 15 minutes. Concurrently N2 gas was bubbled through a solution of 0.530 gm of benzoyl peroxide (2.19 mmole) in 5 mL of DMF for 15 minutes. After N2 deoxygenation, the monomer solution and 2.5 mL of the initiator solution were mixed and placed in a dropping funnel with a pressure equalising tube. The dropping funnel was fitted onto a 100 mL round bottom flask containing 10 gm of kieselguhr. The system was evacuated by means of a water aspirator pump for 5 minutes. The solution was then dropped into the kieselguhr in one portion. With the pump still operating the apparatus was picked up and shaken gently to ensure an even distribution of solution in the kieselguhr. After 3 minutes of shaking the apparatus was closed to the vacuum and N2 was allowed in. The flask of the apparatus was submerged in a 60° C. water bath for 20 minutes. After 17 hours at room temperature the product was collected on a sinter and was washed with DMF and 0.05 M Tris (aq). The material ws then forced through a 700 μm sieve using hand pressure and washing with 0.05 M Tris. The beads were collected and the fines were removed by decantation using 0.05 M Tris. The resin was then washed with DMF and Et2O and was dried over SiO2 under vacuum. Yield: 11.84 gm. Polymer content 22.2%.

1. customN2 gas was bubbled through the solution for 15 minutes
2. customplaced in a dropping funnel with a pressure
3. customThe dropping funnel was fitted onto a 100 mL round bottom flask
4. additioncontaining 10 gm of kieselguhr
5. customThe system was evacuated by means of a water aspirator pump for 5 minutes
6. additionThe solution was then dropped into the kieselguhr in one portion
7. stirringAfter 3 minutes of shaking the apparatus
8. customwas closed to the vacuum and N2
9. customwas submerged in a 60° C.
10. customfor 20 minutes
11. customAfter 17 hours at room temperature the product was collected on a sinter
12. washwas washed with DMF and 0.05 M Tris (aq)
13. washwashing with 0.05 M Tris
14. customThe beads were collected
15. customthe fines were removed by decantation
16. washThe resin was then washed with DMF and Et2O
17. customwas dried over SiO2 under vacuum