HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 2-((2-Benzoylphenylthio)methyl)-2-ethylhexanal
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 2-Mercaptobenzophenone | HCID 3499713 | — |
| Edukt | 2-Ethyl-2-(mesyloxymethyl)hexanal | HCID 11572217 | — |
| Lösungsmittel | Diglyme | HCID 8150 | — |
| Produkt | 2-((2-Benzoylphenylthio)methyl)-2-ethylhexanal | HCID 11602826 | 58% |
Reaktionsschritte
A mixture of 31 g (0.144 mol) of 2-mercaptobenzophenone, prepared according to the procedure described in WO 93/16055, 24.4 g (0.1 mole) of 2-ethyl-2-(mesyloxymethyl)-hexanal (1), 14.8 g (0.146 mole) of triethylamine, and 80 mL of 2-methoxyethyl ether was held at reflux for 24 h. The reaction mixture was poured into 3N HCl and extracted with 300 mL of methylene chloride, The methylene chloride layer was washed with 300 mL of 10% NaOH, dried over MgSO4 and concentrated in vacuo to remove 2-methoxyethyl ether. The residue was purified by HPLC (10% EtOAc-hexane) to give 20.5 g (58%) of 2 as an oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06642268B2 |
| Quelldatensatz | uspto-grants-2003_11 |
| ORD ID | ord-3ba2a7f111dd4316b2eab3ac37c46b53 |
| Quellennotiz | uspto-grants-2003_11 |