반응 #2271667

반응 방정식

H2O

3-(4- methyl-1-piperazinyl)-1-phenylsulfonyl-1H-indazole

K2CO3

cyanogen bromide

→

4-[1-(Phenylsulfonyl)-1H-indazol-3-yl]-1-piperazinecarbonitrile

용매

dimethylsulfoxide

DMSO

반응 조건

후처리

1. 1
   기타The solid, which precipitated from solution
2. 2
   여과was collected by filtration
3. 3
   세척was washed well with H2O affording 168 g (68%) of product
4. 4
   기타A 5.2 g sample was recrystallized twice with ethanol-H2O yielding 4.0 g of 4-[1-(phenylsulfonyl)-1H-indazol-3-yl]-1-piperazinecarbonitrile, m.p.=178°-180° C.

실험 절차

To a stirred mixture of 3-(4- methyl-1-piperazinyl)-1-phenylsulfonyl-1H-indazole (237 g, 0.67 mole), K2CO3 (102 g, 0.74 mole) and dimethylsulfoxide (DMSO, 2000 ml), under nitrogen, was added cyanogen bromide (72 g, 0.68 mmol) dissolved in DMSO (525 ml). The reaction was stirred at ambient temperature for 5.5 hours and was then poured into H2O (7 l). The solid, which precipitated from solution, was collected by filtration and was washed well with H2O affording 168 g (68%) of product. A 5.2 g sample was recrystallized twice with ethanol-H2O yielding 4.0 g of 4-[1-(phenylsulfonyl)-1H-indazol-3-yl]-1-piperazinecarbonitrile, m.p.=178°-180° C.

출처