HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → 6,7-Difluoro-1-(2-fluoro-4-iodo-phenyl)-4-methoxy-1,3-dihydro-benzoimidazol-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | 5,6-difluoro-N1-(2-fluoro-4-iodophenyl)-3-methoxybenzene-1,2-diamine | HCID 53260966 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | 6,7-Difluoro-1-(2-fluoro-4-iodo-phenyl)-4-methoxy-1,3-dihydro-benzoimidazol-2-one | HCID 59386368 | 89.5% |
Reaction Steps
1,1′-Carbonyldiimidazole (4.68 g, 288 mmol) was added portion wise to a solution of 3,4-difluoro-N2-(2-fluoro-4-iodo-phenyl)-6-methoxy-benzene-1,2-diamine (I-5a: 6.3 g, 144 mmol) in DCM (60 mL) and the resulting mixture was stirred at room temperature overnight. The reaction was monitored by TLC (50% ethyl acetate in hexane). The reaction mixture was filtered, the residue was washed with DCM and dried under reduced pressure to afford 6.0 g of the product (89.5% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08614239B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-56ca29b17cb44bd5a7a7c9f0043204ea |
| Source note | uspto-grants-2013_12 |