Water → HCID 15413152, compound

Participants

Reaction Conditions

Reaction Steps

Subsequently, N,N'-bis(3-sulfopropyl)ethylenediamine (5 g, 0.016 mol), water (30 g), and acetone (13 g) were placed in a four-necked flask. The pH of the contents was adjusted to 8.5 with an aqueous 4N NaOH solution. The flask was cooled to 10° C., and caprylic chloride (5.3 g, 0.033 mol) was added dropwise. Since pH falls as the reaction proceeds, an aqueous 4N NaOH solution was added if necessary to maintain the pH between 9 and 10. When the caprylic chloride had been completely added, the mixture was stirred for 1 hour. Water was removed using an evaporator while the mixture underwent azeotropic distillation with ethanol. Thereafter, water (250 g) was added and the mixture was filtered to remove insoluble matter. The residue was desalted by electrodialysis and then freeze-dried to obtain 3.0 g of disodium 4,7-dioctanoyl-4,7-diazadecane-1,10-disulfonate (separation yield: 31 wt %). Mass analysis (FAB ionization method) m/z: 601(M+H+), m=C24H46S2O8N2Na2.

Provenance & Evidence