反応 #74141

反応方程式

cesium carbonate

2-fluoro-pyridyl boronic acid

4-iodo-1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazole

→

2-fluoro-4-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]pyridine

溶媒

dioxane

water

反応条件

後処理

1. 1
   ろ過The mixture was then filtered through a celite pad
2. 2
   その他the filtrate evaporated under reduced pressure
3. 3
   workup.DISSOLUTIONThe residue was re-dissolved with dichloromethane
4. 4
   洗浄washed with water
5. 5
   乾燥The organic layer was dried over sodium sulphate
6. 6
   その他evaporated
7. 7
   その他680 mg (73%) of the title compound crystallized from diethylether

実験手順

1 g (2.3 mmol) of 4-iodo-1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazole (prepared as described in Example 27) were dissolved in a mixture of 20 ml of dioxane and 5 ml of water in a nitrogen atmosphere. 750 mg (2.3 mmol) of cesium carbonate, 350 mg (0.3 mmol) of palladium tetrakis and 486 mg (3.45 mmol) of 2-fluoro-pyridyl boronic acid were added and the reaction stirred at 100° C. for 4 hours. The mixture was then filtered through a celite pad and the filtrate evaporated under reduced pressure. The residue was re-dissolved with dichloromethane and washed with water. The organic layer was dried over sodium sulphate and evaporated. 680 mg (73%) of the title compound crystallized from diethylether.

出典