反応 #10869

反応方程式

thiocarbonyldiimidazole

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

→

1-(4-isothiocyanatophenyl)-4-methylpiperazine

収率 83.0%

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   workup.ADDITION4.78 g, 25.0 mmol) was added over a period of 30 min
2. 2
   その他The cooling bath was removed
3. 3
   温度The mixture was cooled to 0° C.
4. 4
   workup.ADDITIONice-water was added
5. 5
   workup.WAITAfter 30 min
6. 6
   抽出the mixture was extracted with ether (3×200 mL)
7. 7
   乾燥dried (Na2SO4)
8. 8
   ろ過filtered
9. 9
   その他evaporated

実験手順

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.

出典