반응 #10890

반응 방정식

4-[4-(isobutyl)-1-piperazinyl]benzenamine

thiocarbonyldiimidazole

→

1-(4-Isothiocyanatophenyl)-4-(1-isobutyl)piperazine

수율 87.0%

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 (700 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-(isobutyl)-1-piperazinyl]benzenamine (7.8 g, 33.4 mmol) (from Step B above) in N,N-dimethylformamide (75 mL) was added dropwise over 20 min to a cooled (−15° C.) solution of thiocarbonyldiimidazole (5.97 g, 33.5 mmol) (Aldrich) in N,N-dimethylformamide (25 mL). After the addition was complete, the mixture was stirred at −15° C. for 20 min, the cooling bath was removed and the solution was stirred for 1 h. Ice-water (700 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-(1-isobutyl)piperazine (8 g, 87%)

출처