Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | 1,4,7-Tris(carboxymethyl)-1,4,7,10-tetraazacyclododecane | HCID 107830 | — |
| Edukt | Ethyl {4-[(oxiran-2-yl)methoxy]phenyl}acetate | HCID 13324440 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | HCID 15017882 | HCID 15017882 | — |
Reaktionsschritte
10 g (28.87 mmol) of 1,4,7-triscarboxymethyl-1,4,7,10-tetraazacyclododecane (=DO3A) and 12.99 g (51.96 mmol) of 2,3-epoxy-1-[4-(2-ethoxycarbonylmethyl)-phenoxy]-propane are added in 80 ml of dioxane/60 ml of water and adjusted to pH 13 with 6N potassium hydroxide solution. It is stirred for 12 hours at room temperature. Then, it is refluxed for 2 hours. It is adjusted with 5N hydrochloric acid to pH 7 and evaporated to dryness in a vacuum. The residue is absorptively precipitated in 200 ml of ethanol/50 ml of chloroform at 60° C. The precipitated potassium chloride is filtered off and the filtrate is concentrated by evaporation in a vacuum. The residue is purified on a reversed-phase column (RP-18, washing with water, then elution with tetrahydrofuran/water=2:1). The main fractions are concentrated by evaporation in a vacuum.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US05871709 |
|---|
| Quelldatensatz | uspto-grants-1999_02 |
|---|
| ORD ID | ord-646365b070024a4788205eac16673c01 |
|---|
| Quellennotiz | uspto-grants-1999_02 |
|---|