반응 #10872

반응 방정식

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

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

Thiocarbonyl diimidazole

→

1-(2-fluoro-4-isothio-cyanatophenyl)-4-methylpiperazine

용매

N,N-dimethylformamide

N,N-dimethylformamide

반응 조건

후처리

1. 1
   기타the cooling bath was removed
2. 2
   workup.ADDITIONIce-water was then added (100 mL)
3. 3
   추출the mixture was extracted with ether (3×200 mL)
4. 4
   건조The combined ether layers were dried (MgSO4)
5. 5
   여과filtered
6. 6
   기타evaporated

실험 절차

Thiocarbonyl diimidazole (3.00 g, 3.53 mmol) (Aldrich) was dissolved in N,N-dimethylformamide (10 mL) and the solution was cooled to −10° C. (ice/acetone bath). A solution of 3-fluoro-4-(4-methyl-1-piperazinyl) benzenamine (2.26 g, 10.8 mmol) (from Step B above) in N,N-dimethylformamide (30 mL) was added over a period of 30 minutes, then the cooling bath was removed and the solution was stirred overnight. Ice-water was then added (100 mL) and the mixture was extracted with ether (3×200 mL). The combined ether layers were dried (MgSO4), filtered, and evaporated to give 1-(2-fluoro-4-isothio-cyanatophenyl)-4-methylpiperazine as a yellow oil that solidified on standing (3.88 g, 92%).

출처