Reaktion #65160

Reaktionsgleichung

1-(phenylmethyl)piperidine-4-thiol

chloroacetone

sodium carbonate

→

4-[(2-oxopropyl)thio]-1-(phenylmethyl)piperidine

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe insoluble material is filtered off
2. 2
   Waschenwashed with toluene
3. 3
   EinengenAfter concentration
4. 4
   Waschenwashed with dilute sodium hydroxide
5. 5
   TrocknenAfter drying over sodium sulfate
6. 6
   Einengenthe solution is concentrated

Vorschrift

A suspension of 1-(phenylmethyl)piperidine-4-thiol (70 g, prepared in Example 1), chloroacetone (26.9 ml), sodium carbonate (71.6 g) and tetrabutylammonium iodide (31.2 g) in toluene (350 ml) is stirred at room temperature for 4 hours. The insoluble material is filtered off and washed with toluene. After concentration, the filtrate is taken up in dichloromethane and washed with dilute sodium hydroxide and then with a saturated aqueous solution of sodium chloride. After drying over sodium sulfate, the solution is concentrated to give 4-[(2-oxopropyl)thio]-1-(phenylmethyl)piperidine (82.2 g) in the form of an oil, which is sufficiently pure to be used in the next step.

Quelle