HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
N-Methylmorpholine N-oxide monohydrate → 5-(3,5-Difluorobenzoyl)-2-fluorobenzonitrile
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | N-Methylmorpholine N-oxide monohydrate | HCID 2724197 | — |
| Edukt | 5-((3,5-Difluorophenyl)(hydroxy)methyl)-2-fluorobenzonitrile | HCID 68671560 | — |
| Katalysator | HCID 178419074 | HCID 178419074 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 5-(3,5-Difluorobenzoyl)-2-fluorobenzonitrile | HCID 68671472 | 77% |
Reaktionsschritte
A mixture of 5-[(3,5-Difluoro-phenyl)-hydroxy-methyl]-2-fluoro-benzonitrile (2.68 g, 10.2 mmol), 4-methylmorpholine N-oxide monohydrate (2.02 g, 15 mmol) and tetrapropylammonium perruthenate (35 mg, 0.1 mmol) in dry dichloromethane (50 mL) was stirred at room temperature for 2 hours. The reaction mixture was evaporated and the residue redissolved in ethyl acetate. The organic phase was washed with 10% sodium bisulphite and saturated ammonium chloride, dried and evaporated. Purification of the crude by chromatography over silica gel (EtOAc/hexane) afforded 2.05 g of the title compound (77% yield).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09102662B2 |
| Quelldatensatz | uspto-grants-2015_08 |
| ORD ID | ord-a6413daf7a2d46ba85dd4ec0ffbc9114 |
| Quellennotiz | uspto-grants-2015_08 |