HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diethyl Ether → 3-(2,4-Dichloro-5-fluorophenyl)-3-oxopropanenitrile
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diethyl Ether | HCID 3283 | — |
| Edukt | Acetonitrile | HCID 6342 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | Benzoic acid, 2,4-dichloro-5-fluoro-, ethyl ester | HCID 13630722 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 3-(2,4-Dichloro-5-fluorophenyl)-3-oxopropanenitrile | HCID 13630721 | 34,5% |
Reaktionsschritte
A mixture of 47.4 g of ethyl 2,4-dichloro-5-fluoro-benzoate and 8.2 g of anhydrous acetonitrile are added dropwise to a suspension of 6.1 g of 80% strength sodium hydride in 100 ml of anhydrous tetrahydrofuran under reflux in the course of about 1 hour. The mixture is heated at the boiling point under reflux for a further hour and cooled to room temperature, and 150 ml of ether are added. The precipitate is filtered off with suction and dissolved in 50 ml of ice-water and the solution is acidified to pH=6 with 10% strength hydrochloric acid. The precipitate is filtered off cold with suction, rinsed with ice-water and dried in vacuo at 40° C. 16 g of 2,4-dichloro-5-fluoro-benzoylacetonitrile of melting point 96°-98° C. are obtained.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04680401 |
| Quelldatensatz | uspto-grants-1987_07 |
| ORD ID | ord-ae5f28bc56cf4ad582893c7a6f329b85 |
| Quellennotiz | uspto-grants-1987_07 |