反応 #4725

反応方程式

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

溶媒

THF

反応条件

後処理

1. 1
   その他After removal of the THF
2. 2
   その他by evaporation
3. 3
   洗浄the solid residue is washed with ether
4. 4
   workup.DISSOLUTIONdissolved in 30 ml of ethanol
5. 5
   温度with heating
6. 6
   workup.ADDITION1 ml of 30% hydrogen peroxide is added
7. 7
   ろ過The sulphur which separates is filtered off
8. 8
   濃縮the filtrate is concentrated by evaporation
9. 9
   その他the oily residue is purified by preparative layer chromotography

実験手順

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.

出典