반응 #10869

반응 방정식

thiocarbonyldiimidazole

4-(4-methyl-1-piperazinyl)benzenamine

→

1-(4-isothiocyanatophenyl)-4-methylpiperazine

수율 83.0%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   workup.ADDITION4.78 g, 25.0 mmol) was added over a period of 30 min
2. 2
   기타The cooling bath was removed
3. 3
   온도The mixture was cooled to 0° C.
4. 4
   workup.ADDITIONice-water was added
5. 5
   workup.WAITAfter 30 min
6. 6
   추출the mixture was extracted with ether (3×200 mL)
7. 7
   건조dried (Na2SO4)
8. 8
   여과filtered
9. 9
   기타evaporated

실험 절차

A mixture of thiocarbonyldiimidazole (4.46 g, 25.0 mmol) (Aldrich) and N,N-dimethylformamide (20 mL) was cooled to about −15° C. and a solution of 4-(4-methyl-1-piperazinyl)benzenamine (prepared according to the procedure of Chong, W. K. et al. WO9921845; 4.78 g, 25.0 mmol) was added over a period of 30 min. The cooling bath was removed and the mixture was stirred for 1 h. The mixture was cooled to 0° C. and ice-water was added. After 30 min, the mixture was extracted with ether (3×200 mL), dried (Na2SO4), filtered, and evaporated to give 1-(4-isothiocyanatophenyl)-4-methylpiperazine (4.84 g, 83%) as a pale purple solid.

출처