HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Sulfite → Methyl 2-bromo-3,5-dimethoxybenzoate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Sulfite | HCID 24437 | — |
| Edukt | N-bromobutanimide | HCID 67184 | — |
| Edukt | Methyl 3,5-Dimethoxybenzoate | HCID 75074 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | Methyl 2-bromo-3,5-dimethoxybenzoate | HCID 11391696 | 93% |
Reaktionsschritte
3,5-Dimethoxy-benzoic acid methyl ester (4.0 g) was dissolved in MeCN (28 mL), and NBS (4.4 g) was added at 0° C. After stirring at room temperature for 3 hours, saturated Na2SO3 (15 mL) was added. The mixture was evaporated under vacuum and extracted with ether (1×, 500 mL). After the solvent was removed, the crude material was subjected to silica gel chromatography using effluent of 10-40% ethyl acetate and hexanes. The fractions containing product were combined and the solvent was removed under reduced pressure to provide 2-bromo-3,5-dimethoxy-benzoic acid methyl ester (5.2 g, 93%) as a clear oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08822430B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-d4675f1f3d29452e935305b45e3aeff0 |
| Quellennotiz | uspto-grants-2014_09 |