Реакция #4725

Уравнение реакции

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

Растворители

THF

Условия реакции

Обработка

1. 1
   ДругоеAfter removal of the THF
2. 2
   Другоеby evaporation
3. 3
   Промывкаthe solid residue is washed with ether
4. 4
   workup.DISSOLUTIONdissolved in 30 ml of ethanol
5. 5
   Температураwith heating
6. 6
   workup.ADDITION1 ml of 30% hydrogen peroxide is added
7. 7
   ФильтрацияThe sulphur which separates is filtered off
8. 8
   Концентрированиеthe filtrate is concentrated by evaporation
9. 9
   Другоеthe oily residue is purified by preparative layer chromotography

Методика

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.

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