反応 #166649

反応方程式

3-iodo-1-((6-methylpyridin-3-yl)methyl)-4-nitro-1H-indazole

1,10-phenanthroline

potassium fluoride

methanol

→

3-methoxy-1-((6-methylpyridin-3-yl)methyl)-4-nitro-1H-indazole

収率 66.0%

溶媒

toluene

反応条件

後処理

1. 1
   その他was purged with argon
2. 2
   温度heated
3. 3
   温度at reflux for 14 hours
4. 4
   温度After cooling
5. 5
   ろ過the mixture was filtered through glass fiber
6. 6
   ろ過filter paper
7. 7
   濃縮concentrated under reduced pressure
8. 8
   その他purified by silica gel chromatography (5-25% EtOAc in hexanes)

実験手順

A mixture of 3-iodo-1-((6-methylpyridin-3-yl)methyl)-4-nitro-1H-indazole (0.520 g, 1.32 mmol), 1,10-phenanthroline (0.238 g, 1.32 mmol), copper iodide (0.251 g, 1.32 mmol) and potassium fluoride (40% on alumina) (1.05 g, 7.26 mmol) in methanol (2.7 mL) and toluene (13 mL) was purged with argon and heated at reflux for 14 hours. After cooling, the mixture was filtered through glass fiber filter paper, concentrated under reduced pressure and purified by silica gel chromatography (5-25% EtOAc in hexanes) to give 3-methoxy-1-((6-methylpyridin-3-yl)methyl)-4-nitro-1H-indazole (0.260 g, 66% yield) as a brown gum.

出典