HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sulfuric Acid → 3-(4,4-Dimethyl-cyclohex-1-enyl)-propionic acid butyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sulfuric Acid | HCID 1118 | — |
| Edukt | 8,8-Dimethyl-1-oxa-spiro[4.5]decan-2-one | HCID 13409124 | — |
| Lösungsmittel | 1-Butanol | HCID 263 | — |
| Produkt | 3-(4,4-Dimethyl-cyclohex-1-enyl)-propionic acid butyl ester | HCID 23655838 | — |
Reaktionsschritte
The crude 8,8-dimethyl-1-oxa-spiro[4.5]decan-2-one (40.2 g, 0.22 mol) was introduced into a 250 ml three necked round bottom flask together with butanol (23 g) and concentrated H2SO4 (0.5 g). Temperature was risen to 140° C. and during 8 hours fresh butanol (42.9 g) was introduced, while collecting a mixture of butanol/water. The reaction mixture was cooled to room temperature and toluene (66 g) and water (66 g) were added. The organic phase was washed with NaHCO3 and water to yield after concentration 51.42 g of the desired compound. Flash distillation (68°–70° C., 0.2 hPa) led to 35.0 g of butylester (overall yield: 47%; GC purity: 96.0%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06933265B2 |
| Quelldatensatz | uspto-grants-2005_08 |
| ORD ID | ord-0d16dd0ef4a845798ff4baff7b4ef04d |
| Quellennotiz | uspto-grants-2005_08 |