HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 70153777, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-Chloro-2,5-difluorobenzonitrile | HCID 11275302 | — |
| Reactant | HCID 86759700 | HCID 86759700 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 70153777 | HCID 70153777 | 73% |
Reaction Steps
The product of step (b) (277 mg, 1.15 mmol) and 4-chloro-2,5-difluorobenzonitrile (199 mg, 1.15 mmol) were dissolved in dimethylformamide (10 ml) and sodium hydride (60%, 48 mg, 1.2 mmol) added in one portion. The reaction was stirred for 2 h at room temperature then quenched with aqueous saturated ammonium chloride solution (30 ml) and extracted with ethyl acetate (3×60 ml). The combined organic extracts were washed with water (3×20 ml), dried (sodium sulphate) and evaporated iii vacuo. The residue was chromatographed on flash silica, eluting with hexane:ethyl acetate (3:1), to give the title compound as a white crystalline solid (330 mg, 73%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06887871B2 |
| Source dataset | uspto-grants-2005_05 |
| ORD ID | ord-31020b2b24334142b77c80e5b5e6d693 |
| Source note | uspto-grants-2005_05 |