Reaktion #65159
ord-e37be0e885d140fa8bbeac76e7a1f573
Reaktionsgleichung
Sodium methylate
1-methylpiperidine-4-thiol
chloroacetone
→
1-methyl-4-[(2-oxopropyl)thio]piperidine
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Filtrationthe precipitate is filtered off
- 2Einengenthe filtrate is concentrated
- 3Sonstigechromatographed on silica gel (eluent
Vorschrift
Sodium methylate (5.9 g) is added in portions to a solution of 1-methylpiperidine-4-thiol (14 g) in anhydrous tetrahydrofuran (100 ml) at room temperature. After 2 hours at this temperature, chloroacetone (8.8 ml) is added dropwise. After 24 hours, the precipitate is filtered off and the filtrate is concentrated and chromatographed on silica gel (eluent: ethyl acetate, then ethanol) to give 1-methyl-4-[(2-oxopropyl)thio]piperidine (11.5 g) in the form of an oil.