Réaction #818315

Équation de réaction

sodium methoxide

triethylenetetramine tetrahydrochloride

→

triethylenetetramine

Rendement 95.0%

Solvants

ethanol

methanol

Conditions de réaction

Traitement

1. 1
   FiltrationThe reaction mixture is filtered
2. 2
   Autrethe solvent is evaporated
3. 3
   workup.DISSOLUTIONthe product is dissolved in tert-butylmethylether
4. 4
   Filtrationagain filtered
5. 5
   workup.DISSOLUTIONdissolved

Mode opératoire

In one embodiment about 4 equivalents of sodium methoxide are mixed with about 1 equivalent of triethylenetetramine tetrahydrochloride in a mixture of methanol and ethanol, for example. The reaction mixture is filtered, the solvent is evaporated, and the product is dissolved in tert-butylmethylether and again filtered and dissolved, giving triethylenetetramine in yield greater than about 95%. The triethylenetetramine is dissolved in about 2.0 equivalents of concentrated hydrochloric acid. Less than about 2 equivalents of concentrated hydrochloric acid may also be used. Ethanol is added and triethylenetetramine dihydrochloride precipitates in yield greater than about 86%. Purity of triethylenetetramine dihydrochloride so produced is about 100%, as determined using the methods set forth in USP27-NF22 (page 1890) for analysis of trientine, with less than about 10 ppm heavy metals as determined by USP <231> II.

Source