تفاعل #4725

معادلة التفاعل

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

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   أخرىAfter removal of the THF
2. 2
   أخرىby evaporation
3. 3
   غسيلthe solid residue is washed with ether
4. 4
   workup.DISSOLUTIONdissolved in 30 ml of ethanol
5. 5
   درجة الحرارةwith heating
6. 6
   workup.ADDITION1 ml of 30% hydrogen peroxide is added
7. 7
   ترشيحThe sulphur which separates is filtered off
8. 8
   تركيزthe filtrate is concentrated by evaporation
9. 9
   أخرىthe oily residue is purified by preparative layer chromotography

الإجراء التجريبي

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.

المصدر