HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 2-(4-Chlorophenyl)-2-(4-nitrophenyl)-1,3-dioxolane
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Toluene | HCID 1140 | — |
| Edukt | p-Toluenesulfonic acid | HCID 6101 | — |
| Edukt | 4-Chloro-4'-nitrobenzophenone | HCID 347771 | — |
| Lösungsmittel | Ethylene Glycol | HCID 174 | — |
| Produkt | 2-(4-Chlorophenyl)-2-(4-nitrophenyl)-1,3-dioxolane | HCID 15489626 | 91% |
Reaktionsschritte
Toluene (1900 ml) was stirred in a round-bottom flask (51) using a water separator. (4-Chlorophenyl)(4-nitrophenyl)methanone (250 g) was added portionwise. p-Toluene-sulfonic acid (54.5 g) was added portionwise. Ethylene glycol (237.5 g) was poured out into the mixture. The mixture was stirred and refluxed for 48 hours. The solvent was evaporated. The residue was dissolved into ethyl acetate (5 l) and washed twice with a K2CO3 10% solution. The organic layer was separated, dried (MgSO4), filtered and the solvent was evaporated. The residue was stirred in DIPE, filtered off and dried (vacuum, 40° C., 24 hours), yielding 265 g (91%) of 2-(4-chlorophenyl)-2-(4-nitrophenyl)-1,3-dioxolane (interm. 5-a).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06169096A |
| Quelldatensatz | uspto-grants-2001_01 |
| ORD ID | ord-f1a653b03e0c40d1ae8146d7d9fbdcab |
| Quellennotiz | uspto-grants-2001_01 |