반응 #65160

반응 방정식

1-(phenylmethyl)piperidine-4-thiol

chloroacetone

sodium carbonate

→

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

용매

toluene

반응 조건

후처리

1. 1
   여과The insoluble material is filtered off
2. 2
   세척washed with toluene
3. 3
   농축After concentration
4. 4
   세척washed with dilute sodium hydroxide
5. 5
   건조After drying over sodium sulfate
6. 6
   농축the solution is concentrated

실험 절차

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.

출처