반응 #4725

반응 방정식

benzoyl isothiocyanate

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

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

용매

THF

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후처리

1. 1
   기타After removal of the THF
2. 2
   기타by evaporation
3. 3
   세척the solid residue is washed with ether
4. 4
   workup.DISSOLUTIONdissolved in 30 ml of ethanol
5. 5
   온도with heating
6. 6
   workup.ADDITION1 ml of 30% hydrogen peroxide is added
7. 7
   여과The sulphur which separates is filtered off
8. 8
   농축the filtrate is concentrated by evaporation
9. 9
   기타the oily residue is purified by preparative layer chromotography

실험 절차

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.

출처