HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 59470601, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Dimethylacetamide | HCID 31374 | — |
| Reactant | Propanediol | HCID 134919 | — |
| Reactant | HCID 53903191 | HCID 53903191 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 59470601 | HCID 59470601 | — |
Reaction Steps
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).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08202511B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-9de2866bb0c1419ca7946ef3cf685deb |
| Source note | uspto-grants-2012_06 |