Reaktion #54172

Reaktionsgleichung

3-methylpiperidine

2-mercaptobenzothiazole

sodium hydroxide

sodium hypochlorite

→

1-(2-benzothiazolylthio)-3-methyl-piperidine

Ausbeute 95.5%

Lösungsmittel

ethyl acetate

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto form a solution
2. 2
   Sonstigeis kept below 70° C
3. 3
   workup.WAITto stand at the same temperature for 1 hour
4. 4
   ExtraktionThe ethyl acetate extract
5. 5
   Waschenis washed with water
6. 6
   workup.DISTILLATIONdistilled under reduced pressure

Vorschrift

In a 500 ml volume flask, there are charged 2-mercaptobenzothiazole (UV absorption spectrum: 329 mμ) (41.28 g), sodium hydroxide (10 g) and water (180 ml), and the resultant mixture is stirred to form a solution. After the addition of 3-methylpiperidine (27.2 g) to the resulting solution, a 15 % by volume aqueous solution of sodium hypochlorite (138.5 ml) is dropwise added thereto in 2 hours, during which the inner temperature is kept below 70° C. The reaction mixture is allowed to stand at the same temperature for 1 hour and then shaken with ethyl acetate (150 ml). The ethyl acetate extract is washed with water and distilled under reduced pressure to give 1-(2-benzothiazolylthio)-3-methyl-piperidine (62.3 g).

Quelle