N'-[2-[2-(2-aminoethylamino)ethylamino]ethyl]ethane-1,2-diamine;hydrochloride

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 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"). The methanolic KOH was filtered off on a Buchner funnel 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 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 added to a flask 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 wash fractions