HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1-Bromo-4-fluoro-2-methyl-5-nitrobenzene → 5-Bromo-2-fluoro-4-methylaniline
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1-Bromo-4-fluoro-2-methyl-5-nitrobenzene | HCID 10036983 | — |
| Edukt | HCID 178418361 | HCID 178418361 | — |
| Katalysator | Nickel | HCID 935 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | 5-Bromo-2-fluoro-4-methylaniline | HCID 46739114 | 63,2% |
Reaktionsschritte
Combine crude 1-bromo-4-fluoro-2-methyl-5-nitrobenzene (32.4 g, 138 mmol), ethanol (100 mL) and Raney Nickel (1.00 g, 17.04 mmol) in a shaker flask. Charge the flask with hydrogen (275 kPa) and agitate until the absorption of hydrogen ceases. De-pressurize the reaction vessel, remove the catalyst by filtration, and evaporate the filtrate to dryness. Add MTBE, then filter again and evaporate the filtrate. Stir residue in hexanes. Collect the solids by filtration, wash with cold hexanes and dry in vacuo to provide the title compound (17.8 g, 63% yield) as a dark solid. MS (m/z): 204.0 (M+1)/206.0 (M+3).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09334267B2 |
| Quelldatensatz | uspto-grants-2016_05 |
| ORD ID | ord-ee685ee613564d3fa6d76b9da194d191 |
| Quellennotiz | uspto-grants-2016_05 |