反応 #595381

反応方程式

NaHSO3

4-fluoroindazole

I2

KOH

→

title compound

4-fluoro-3-iodo-1H-indazole

溶媒

DMF

反応条件

後処理

1. 1
   抽出extracted with EtOAc (200 mL*3)
2. 2
   洗浄The combined organic layers were washed with H2O and brine
3. 3
   乾燥dried over Na2SO4
4. 4
   濃縮concentrated
5. 5
   洗浄The crude solid was washed with PE

実験手順

To a solution of 4-fluoroindazole A-1 (5.00 g, 36.7 mmol) in DMF (80 mL) was added I2 (18.6 g, 73.5 mmol) and KOH (7.73 g, 134 mmol) successively at rt. After 2 h, the reaction mixture was poured into aq. 10% NaHSO3 (200 mL) and extracted with EtOAc (200 mL*3). The combined organic layers were washed with H2O and brine, dried over Na2SO4, and concentrated. The crude solid was washed with PE to give the title compound as a yellow solid. LCMS (ESI) calc'd for C7H5FIN2 [M+H]+: 262.9. found: 262.9.

出典