HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 67073865, compound → HCID 67074292, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 67073865 | HCID 67073865 | — |
| Solvent | Tetrahydrofuran ethanol | HCID 21873804 | — |
| Product | HCID 67074292 | HCID 67074292 | 65.9% |
Reaction Steps
1.6 g crude N-(3-{5-fluoro-3-[(2-fluoro-4-iodophenyl)amino]-2-nitrophenoxy}-2-methylphenyl)-ethanesulfonamide (2.7 mmol, 1 eq.) were dissolved in 40 mL THF/EtOH 1:1 and treated with 3.1 g stannous chloride dihydrate (SnCl2 2H2O) (13.6 mmol, 5 eq.) and the resulting mixture was refluxed for 16 h. The reaction mixture was concentrated, the residue quenched with 26% NH3 and extracted with DCM. The combined organic layers were washed with ammonium chloride solution and saturated sodium chloride solution, dried, filtered and concentrated in vacuo. The residue was purified by flash column chromatography to give 996 mg of the target compound (65% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08962606B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-4abf83a4f25b42be804f491998c1f1d9 |
| Source note | uspto-grants-2015_02 |