HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
p-Toluenesulfonic acid → 4-Methoxy-2,2-dimethyl-1,3-benzodioxole
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | p-Toluenesulfonic acid | HCID 6101 | — |
| Edukt | 3-Methoxycatechol | HCID 13622 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Lösungsmittel | Benzene | HCID 241 | — |
| Produkt | 4-Methoxy-2,2-dimethyl-1,3-benzodioxole | HCID 15061094 | — |
Reaktionsschritte
3-methoxycatechol (25 g) was dissolved in benzene, mixed with dimethoxyacetal (35 ml) and a catalytic amount of tosylic acid, and then, heat-refluxed for 6 hours. The resultant was allowed to stand for cooling, alkalified by adding an aqueous sodium hydroxide solution, and extracted with ether. The organic layer was washed with a saturated aqueous sodium chloride solution, dried over manganese sulfate, and evaporated under reduced pressure for removing the solvent. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=99/1) to give Compound IIbv-a (19.4 g, 60.5%) as a white solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06514996B2 |
| Quelldatensatz | uspto-grants-2003_02 |
| ORD ID | ord-6333eb2aab974270b8b7deba206c7a2b |
| Quellennotiz | uspto-grants-2003_02 |