HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 1-((2-Benzoylphenylthio)methyl)cyclohexanecarboxaldehyde
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 2-Mercaptobenzophenone | HCID 3499713 | — |
| Edukt | 1-(Mesyloxymethyl)cyclohexanecarboxaldehyde | HCID 22325261 | — |
| Lösungsmittel | Diglyme | HCID 8150 | — |
| Produkt | 1-((2-Benzoylphenylthio)methyl)cyclohexanecarboxaldehyde | HCID 22325208 | 75,9% |
Reaktionsschritte
A mixture of 69 g (0.303 mole) of 2-mercaptobenzophenone, 82 g (0.303 mole) of mesylate 55, 32 g of triethylamine, and 150 ml of diglyme was stirred and held at reflux for 24 h. The mixture was cooled, poured into dil. HCl and extracted with methylene chloride. The organic layer was washed with 10% NaOH, water, brine, and dried over sodium sulfate and concentrated under vacuum to remove excess diglyme. This was purified by silica gel flush column (5% EtOAc:Hexane) and gave 18.6 g (75.9%) of yellow oil. Proton NMR and mass spectra were consistent with the product.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06420417B1 |
| Quelldatensatz | uspto-grants-2002_07 |
| ORD ID | ord-2f71fdaa36f94a28b4301990659889dc |
| Quellennotiz | uspto-grants-2002_07 |