Reaktion #65159

ord-e37be0e885d140fa8bbeac76e7a1f573

Reaktionsgleichung

C[O-].[Na+]
Sodium methylate
CN1CCC(S)CC1
1-methylpiperidine-4-thiol
CC(=O)CCl
chloroacetone
CC(=O)CSC1CCN(C)CC1
1-methyl-4-[(2-oxopropyl)thio]piperidine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationthe precipitate is filtered off
  2. 2
    Einengenthe filtrate is concentrated
  3. 3
    Sonstigechromatographed 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05418242uspto-grants-1995_05