반응 #10886

반응 방정식

4-[4-(sec-butyl)-1-piperazinyl]benzenamine

thiocarbonyldiimidazole

→

1-(4-isothiocyanatophenyl)-4-(sec-butyl)piperazine

수율 87.1%

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 (800 ml) was added
5. 5
   workup.STIRRINGthe mixture was stirred for 30 min
6. 6
   여과The solid was filtered off
7. 7
   세척washed with water
8. 8
   기타dried under vacuum

실험 절차

A solution of 4-[4-(sec-butyl)-1-piperazinyl]benzenamine (3.5 g, 15 mmol) (from Step B above) in N,N-dimethylformamide (40 mL) was added dropwise over 20 min to a cooled (−15° C.) solution of thiocarbonyldiimidazole (2.68 g, 15.03 mmol) (Aldrich) in N,N-dimethylformamide (15 mL). After the addition was complete, the mixture was stirred at −15° C. for 20 min, then the cooling bath was removed and the solution was stirred for 1 h. Ice-water (800 ml) was added and the mixture was stirred for 30 min. The solid was filtered off and washed with water and dried under vacuum to give 1-(4-isothiocyanatophenyl)-4-(sec-butyl)piperazine (3.6 g, 87%) as a purple solid.

출처