HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
p-Toluenesulfonic acid → Ethanone, 2-bromo-1-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)-
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | p-Toluenesulfonic acid | HCID 6101 | — |
| Edukt | 2-Methoxypropene | HCID 8300 | — |
| Edukt | 2-Bromo-1-(4-hydroxy-3-(hydroxymethyl)phenyl)ethan-1-one | HCID 11334055 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | Ethanone, 2-bromo-1-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)- | HCID 11150315 | 82,5% |
Reaktionsschritte
2-Methoxypropene (10 g) was added over 15 min to a stirred solution of 2-bromo-1-[4-hydroxy-3-(hydroxymethyl)phenyl]ethanone (5 g) and toluene-4-sulphonic acid (0.5 g) in CH2Cl2 (100 ml) at 23°. The mixture was stirred for 3h, filtered through a wad of triethylamine-deactivated silica and evaporated to give an oil. Purification by [FCTS] (300 g) [E] afforded the title compound as an oil (4.8 g) with solidified on cooling. A small sample was crystallised from light petroleum (b.p. 60-80°) to give white crystals m.p. 47-48°.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05243076 |
| Quelldatensatz | uspto-grants-1993_09 |
| ORD ID | ord-c168fac950b8444d8d024b6f43774ded |
| Quellennotiz | uspto-grants-1993_09 |