HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethylformamide → 1-(2-Chloroethyl)-4-(4-fluorobenzoyl)piperidine hydrochloride
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | Thionyl Chloride | HCID 24386 | — |
| Edukt | 4-(4-Fluorobenzoyl)-1-(2-hydroxyethyl)piperidine | HCID 14892165 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 1-(2-Chloroethyl)-4-(4-fluorobenzoyl)piperidine hydrochloride | HCID 67575338 | 96,3% |
Reaktionsschritte
In an atmosphere of dry air, 4-(4-fluorobenzoyl)-1-(2-hydroxyethyl)piperidine (1.96 g, 7.8 mmol) was dissolved in methylene chloride (10 ml) to which, with cooling in an ice bath, were subsequently added dropwise DMF (0.1 ml) and thionyl chloride (2.5 ml, 34.2 mmol). After 7 hours of stirring at room temperature, the solvent was removed by evaporation, and the resulting residue was subjected to azeotropic distillation using benzene (15 ml×2). Thereafter, the thus obtained residue was washed with an ether-methylene chloride (4:1) mixture solution (30 ml) to obtain 2.3 g (96.3%) of the title compound in the form of light beige powder.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05728835 |
| Quelldatensatz | uspto-grants-1998_03 |
| ORD ID | ord-761b0c03342a44cd91f901367699772b |
| Quellennotiz | uspto-grants-1998_03 |