HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Carbon tetrabromide → 1-(Bromomethyl)-2-fluoro-3-methoxybenzene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Carbon tetrabromide | HCID 11205 | — |
| Edukt | Triphenylphosphine | HCID 11776 | — |
| Edukt | 2-Fluoro-3-methoxybenzyl alcohol | HCID 593589 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 1-(Bromomethyl)-2-fluoro-3-methoxybenzene | HCID 26986100 | — |
Reaktionsschritte
Triphenylphosphine (11.1 g) was added to a solution of the subtitle product of step ii) (5.0 g) in DCM (200 ml) followed by the portionwise addition of carbon tetrabromide (14.0 g). The reaction was stirred for 4 h before the addition of further triphenylphosphine (2.0 g) and carbon tetrabromide (2.0 g) and stirring maintained for 1 h. The mixture was concentrated to 30 ml volume and diluted in Et2O (300 ml). The solid precipitate was filtered and washed with Et2O (3×) and the filtrate concentrated in vacuo. The residue was purified by column chromatography (10% Et2O/iso-hexane) to afford the subtitle compound as a clear oil. Yield: 5.2 g.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07582644B2 |
| Quelldatensatz | uspto-grants-2009_09 |
| ORD ID | ord-9f802557b38140a28afce8dfa93633d6 |
| Quellennotiz | uspto-grants-2009_09 |