反応 #2298651

反応方程式

H2O

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

K2CO3

cyanogen bromide

→

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

溶媒

dimethylsulfoxide

DMSO

反応条件

後処理

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

実験手順

To a stirred mixture of 3-(4-methyl-1-piperazinyl)-1-phenylsulfonyl-1H-indazole (237 g, 0.67 mol), K2CO3 (102 g, 0.74 mol) and dimethylsulfoxide (DMSO, 2000 ml), under nitrogen, was added cyanogen bromide (72 g, 0.68 mol) 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 from ethanol-H2O yielding 4.0 g of 4-[1-(phenylsulfonyl)-1H-indazol-3-yl]-1-piperazinecarbonitrile, m.p.=178°-180° C.

出典