HuagongsheHuagongshe Chemistry Print Report · For research reference only
5-Amino-2,4,6-triiodoisophthaloyl dichloride → 2,4,6-triiodo-5-(((2-(1-methylethyl)-1,3-dioxan-5-yl)carbonyl)amino)-1,3-Benzenedicarbonyl dichloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 5-Amino-2,4,6-triiodoisophthaloyl dichloride | HCID 9894858 | — |
| Reactant | 2-(Propan-2-yl)-1,3-dioxane-5-carbonyl chloride | HCID 17882217 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | 2,4,6-triiodo-5-(((2-(1-methylethyl)-1,3-dioxan-5-yl)carbonyl)amino)-1,3-Benzenedicarbonyl dichloride | HCID 19825447 | — |
Reaction Steps
137 g of 5-amino-2,4,6-triiodoisophthaloyl chloride (0.23 mole) are dissolved in 460 ml of DMAC to which are added 110 g (0.57 mole) of 2-isopropyl-1,3-dioxane-5-carboxylic acid chloride. The reaction mixture is stirred under argon at ambient temperature for 4 days. The DMAC is removed in a vacuum. The oil obtained is extracted with 3 l of ethyl acetate and washed twice with 1 l of ice-cold water. The organic phase is dried and concentrated to dryness. The product is crystallized from 200 ml of CH2Cl2. After filtration, 110 g of solid are obtained:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05043152 |
| Source dataset | uspto-grants-1991_08 |
| ORD ID | ord-9e7f88325485421d8187fbf994248911 |
| Source note | uspto-grants-1991_08 |