반응 #48038

반응 방정식

1-(4-chlorophenyl)-5-phenyl-4,5-dihydro-(1H)-pyrazole-3-carboxamidine

HCl

4-fluorophenylsulfonyl chloride

triethylamine

→

N-[(4-fluorophenyl)sulfonyl]-1-(4-chlorophenyl)-5-phenyl-4,5-dihydro-(1H)-pyrazole-3-carboxamidine

수율 54.0%

용매

acetonitrile

반응 조건

후처리

1. 1
   농축After concentration in vacuo
2. 2
   workup.DISSOLUTIONthe residue is dissolved in a mixture of Ethyl acetate and water
3. 3
   기타The Ethyl acetate layer is collected
4. 4
   건조dried over MgSO4
5. 5
   여과filtered
6. 6
   농축concentrated in vacuo
7. 7
   기타The resulting residue is recrystallised from methyl-t-butyl ether

실험 절차

Part B: To a stirred solution of 1-(4-chlorophenyl)-5-phenyl-4,5-dihydro-(1H)-pyrazole-3-carboxamidine.HCl (1.87 gram, 5 mmol) and 4-fluorophenylsulfonyl chloride (0.97 g, 5 mmol) in anhydrous acetonitrile (20 ml) is added triethylamine (2.1 ml, 15 mmol) and the resulting mixture is stirred at room temperature for 16 hours. After concentration in vacuo, the residue is dissolved in a mixture of Ethyl acetate and water. The Ethyl acetate layer is collected, dried over MgSO4, filtered and concentrated in vacuo. The resulting residue is recrystallised from methyl-t-butyl ether to give N-[(4-fluorophenyl)sulfonyl]-1-(4-chlorophenyl)-5-phenyl-4,5-dihydro-(1H)-pyrazole-3-carboxamidine (1.22 gram, 54% yield). Melting point: 200-203.5° C.

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