반응 #10876

반응 방정식

1-acetyl-4-(4-aminophenyl)piperazine

1-acetyl-4-(4-amino-phenyl)piperazine

thiocarbonyldiimidazole

→

1-(acetyl)-4-(4 isothiocyanatophenyl)piperazine

수율 84.0%

용매

N,N-dimethylformamide

N,N-dimethylformamide

반응 조건

후처리

1. 1
   workup.ADDITIONAfter the addition
2. 2
   기타the cooling bath was removed
3. 3
   workup.STIRRINGthe solution was stirred for 1 h
4. 4
   workup.ADDITIONIce-water was added
5. 5
   추출the mixture was extracted with ether (4×50 mL)
6. 6
   세척The combined ether layers were washed with brine
7. 7
   건조dried (MgSO4)
8. 8
   여과filtered
9. 9
   기타evaporated

실험 절차

A solution of 1-acetyl-4-(4-aminophenyl)piperazine (1.0 g, 4.6 mmol) (from Step B above) in N,N-dimethylformamide (10 mL) was added dropwise to a cooled (−15° C.) solution of thiocarbonyldiimidazole (855 mg, 4.8 mmol) in N,N-dimethylformamide (10 mL). After the addition was complete, the mixture was stirred at −15° C. for 30 min, then the cooling bath was removed and the solution was stirred for 1 h. Ice-water was added and the mixture was extracted with ether (4×50 mL). The combined ether layers were washed with brine, dried (MgSO4), filtered, and evaporated to give 1-(acetyl)-4-(4 isothiocyanatophenyl)piperazine (1.0 g, 84%).

출처