HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methanol → HCID 59470601, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methanol | HCID 887 | — |
| Edukt | Dimethylacetamide | HCID 31374 | — |
| Edukt | Propanediol | HCID 134919 | — |
| Edukt | HCID 53903191 | HCID 53903191 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | HCID 59470601 | HCID 59470601 | — |
Reaktionsschritte
Acetic acid [(3,5-bis-chlorocarbonyl-2,4,6-triiodo-phenyl)-methyl-carbamoyl]-methyl ester (16.25 g, 22.9 mmol) and 3-methylamino-1,2,-propanediol (4.42 ml, 45.8 mmol) were stirred in DMA (80 ml) for 72 hours at room temperature. The mixture was diluted with ethyl acetate (150 ml) and washed with ice water/brine (50:50, 20 ml×3). The organics were collected, dried over MgSO4, filtered and evaporated to dryness. The product was purified by silica column chromatography eluting with DCM: methanol to give acetic acid ({3-chlorocarbonyl-5-[(2,3-dihydroxy-propyl)-methyl-carbamoyl]-2,4,6-triiodo-phenyl}-methyl-carbamoyl)-methyl ester (5.42 g, 6.96 mmol).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08202511B2 |
| Quelldatensatz | uspto-grants-2012_06 |
| ORD ID | ord-9de2866bb0c1419ca7946ef3cf685deb |
| Quellennotiz | uspto-grants-2012_06 |