HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Phosphorus tribromide → 3,4-Methylenedioxyphenethyl bromide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Phosphorus tribromide | HCID 24614 | — |
| Edukt | 2-(1,3-Dioxaindan-5-yl)ethan-1-ol | HCID 2759846 | — |
| Lösungsmittel | Carbon Tetrachloride | HCID 5943 | — |
| Produkt | 3,4-Methylenedioxyphenethyl bromide | HCID 12207224 | 121,1% |
Reaktionsschritte
A solution of phosphorus tribromide (8.1 g) in carbon tetrachloride (50 ml) was added dropwise over 30 minutes to a stirred solution of 3,4-methylenedioxyphenethyl alcohol (15.0 g) (see Preparation 5) in carbon tetrachloride (200 ml) and the mixture was heated under reflux for 3 hours, washed sequentially with water (twice), 5M aqueous sodium hydroxide solution and water, dried over magnesium sulphate and evaporated. The residue was purified by chromatography on silica (100 g) using carbon tetrachloride as the eluant. Appropriate fractions were combined and evaporated to give the title compound as a pale yellow oil (8.3 g, 40%), which was characterised by its 1H-NMR spectrum.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05486527 |
| Quelldatensatz | uspto-grants-1996_01 |
| ORD ID | ord-d8498382db174ecc82a5bba16c88d659 |
| Quellennotiz | uspto-grants-1996_01 |