反応 #2298652

反応方程式

4-(1H-indazol-3-yl)-1-piperazinecarbonitrile

NaOH

→

desired compound

収率 73.0%

3-(1-Piperazinyl)-1H-indazole

収率 73.0%

溶媒

H2SO4

反応条件

後処理

1. 1
   温度at reflux for 4.5 hours
2. 2
   温度The reaction was cooled in an ice bath
3. 3
   抽出The basic solution was extracted with ethyl acetate
4. 4
   洗浄The ethyl acetate was washed with H2O
5. 5
   乾燥dried with MgSO4
6. 6
   濃縮concentrated

実験手順

A mixture of 4-(1H-indazol-3-yl)-1-piperazinecarbonitrile (8.0 g, 0.04 mol) and 25% H2SO4 (100 ml) was stirred at reflux for 4.5 hours. The reaction was cooled in an ice bath and made basic by the dropwise addition of 50% NaOH. The basic solution was extracted with ethyl acetate. The ethyl acetate was washed with H2O, dried with MgSO4, and concentrated to afford 5.2 g (73%) of the desired compound, as a solid. The solid was recrystallized twice from toluene to afford 3.0 g of 3-(1-piperazinyl)-1H-indazole, m.p.=153°-155° C.

出典