Potassium Hydroxide → Tetraethylenepentamine

100 Grams of the acid-washed silica was added to 150-200 ml of 2 M potassium hydroxide in methanol and stirred for 5 minutes under vacuum. The methanolic KOH was filtered off on a Buchner funnel, and the silica was rinsed with a small amount of methanol. The silica was added to 5.3 g of cyanogen bromide in 20 ml of acetonitrile on an ice bath with stirring, over a period of 2 minutes. The mixture was allowed to stir for a total of 5 minutes, after which time the excess CNBr/acetonitrile was filtered off on a Buchner funnel. The silica was rinsed quickly with acetonitrile, then added to a flask containing 20 mmoles of tetraethylenepentamine HCl in water at pH 9.0. The mixture was incubated overnight on a shaker at room temperature, after which excess tetraethylenepentamine was removed by filtration on extensive rinsing with 1 mM sodium hydroxide, followed by water, until tetraethylenepentamine was no longer detected in the eluted wash fractions to give tetraethylenepentamine immobilized on silica ("silica/tetren").

1. filtrationThe methanolic KOH was filtered off on a Buchner funnel
2. washthe silica was rinsed with a small amount of methanol
3. additionThe silica was added to 5.3 g of cyanogen bromide in 20 ml of acetonitrile on an ice bath
4. stirringwith stirring, over a period of 2 minutes
5. stirringto stir for a total of 5 minutes
6. filtrationafter which time the excess CNBr/acetonitrile was filtered off on a Buchner funnel
7. washThe silica was rinsed quickly with acetonitrile
8. additionadded to a flask
9. waitThe mixture was incubated overnight on a shaker at room temperature
10. customafter which excess tetraethylenepentamine was removed by filtration
11. washon extensive rinsing with 1 mM sodium hydroxide
12. washwash fractions

ORD record

ord-213ee822932648638e3710fbac8667c8

Source dataset

uspto-grants-1992_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05096724