HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Tetrahydrofuran → 4-[(2,2-Diethoxyethyl)thio]-1-methylpiperidine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Tetrahydrofuran | HCID 8028 | — |
| Edukt | Acetaldehyde, bromo- | HCID 105131 | — |
| Edukt | Sodium Methoxide | HCID 10942334 | — |
| Edukt | 1-Methylpiperidine-4-thiol | HCID 14180391 | — |
| Produkt | 4-[(2,2-Diethoxyethyl)thio]-1-methylpiperidine | HCID 19936607 | — |
Reaktionsbedingungen
| Temperatur | 40 °C |
|---|
Reaktionsschritte
Sodium methylate (18.1 g) is added in portions to a solution of 1-methylpiperidine-4-thiol (22 g) in anhydrous tetrahydrofuran (200 ml). After one hour, the diethyl acetal of bromoacetaldehyde (30.3 ml) is added. After 4 hours at room temperature, the solution is heated for 2 hours at 40° C. The insoluble material is filtered off and rinsed with THF. The filtrate is concentrated and then distilled under reduced pressure to give 4-[(2,2-diethoxyethyl)thio]-1-methylpiperidine (36 g; b.p.=104°-108° C. under 0.05 atm) in the form of an oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05317025 |
| Quelldatensatz | uspto-grants-1994_05 |
| ORD ID | ord-a9638a2874c04bb1b06c240812972e9b |
| Quellennotiz | uspto-grants-1994_05 |