HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 8-iodo-2,3,4,5-tetrahydro-1H-1-benzazepine-2,5-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | methyl 8-iodo-2,5-dioxo-2,3,4,5-tetrahydro-1H-1-benzazepine-4-carboxylate | HCID 58476574 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Water | HCID 962 | — |
| Product | 8-iodo-2,3,4,5-tetrahydro-1H-1-benzazepine-2,5-dione | HCID 58476623 | 99.6% |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
A mixture of methyl 8-iodo-2,5-dioxo-2,3,4,5-tetrahydro-1H-1-benzazepine-4-carboxylate (74 g, 0.2 mol) in DMSO (560 mL) and H2O (16 mL) was heated at 150° C. for 4 h. The reaction mixture was allowed to cool to rt, ice (1.0 L) was added, and the mixture was allowed to stir 12 h. To the flask was added 1N HCl (1.0 L) at 0° C. and the mixture allowed to stir for 3 h. The resulting precipitate was filtered and dried under reduced pressure to afford 8-iodo-3,4-dihydro-1H-1-benzazepine-2,5-dione (60 g, 97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08268992B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-d1c91e1f8944416685dbd768794dd58d |
| Source note | uspto-grants-2012_09 |