Reaktion #4725

Reaktionsgleichung

benzoyl isothiocyanate

N-[2-hydroxy-3-[3-(1-piperidinylmethyl)phenoxy]propyl]-hydrazine carbothioamide

→

N-Benzoyl-N'-[2-hydroxy-3-[3-(1-piperidinylmethyl)phenoxy]propyl]-1,3,4-thiadiazole-2,5-diamine

Lösungsmittel

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter removal of the THF
2. 2
   Sonstigeby evaporation
3. 3
   Waschenthe solid residue is washed with ether
4. 4
   workup.DISSOLUTIONdissolved in 30 ml of ethanol
5. 5
   Temperaturwith heating
6. 6
   workup.ADDITION1 ml of 30% hydrogen peroxide is added
7. 7
   FiltrationThe sulphur which separates is filtered off
8. 8
   Einengenthe filtrate is concentrated by evaporation
9. 9
   Sonstigethe oily residue is purified by preparative layer chromotography

Vorschrift

0.33 g (2 mmol) of benzoyl isothiocyanate are added to 0.68 g (2 mmol) of N-[2-hydroxy-3-[3-(1-piperidinylmethyl)phenoxy]propyl]-hydrazine carbothioamide in 20 ml of THF and the reaction mixture is stirred overnight at room temperature. After removal of the THF by evaporation, the solid residue is washed with ether and dissolved in 30 ml of ethanol with heating, and 1 ml of 30% hydrogen peroxide is added. The sulphur which separates is filtered off, the filtrate is concentrated by evaporation and the oily residue is purified by preparative layer chromotography.

Quelle