反応 #48599

反応方程式

sodium nitrite

4-amino-1H-pyrazole-3-carboxylic acid phenylamide

potassium iodide

→

4-iodo-1H-pyrazole-3-carboxylic acid phenylamide

収率 21.7%

溶媒

acetone

water

hydrochloric acid

ethyl acetate

brine

反応条件

後処理

1. 1
   workup.STIRRINGstirred at room temperature for 90 minutes
2. 2
   洗浄then washed with saturated sodium thiosulphate solution
3. 3
   その他The ethyl acetate layer was separated
4. 4
   乾燥dried (MgSO4)
5. 5
   ろ過filtered
6. 6
   その他evaporated

実験手順

An aqueous solution of sodium nitrite (760 mg) in 2 ml of water was added drop wise to a stirred suspension of 4-amino-1H-pyrazole-3-carboxylic acid phenylamide (2 g; 10 mmol) in concentrated hydrochloric acid (20 ml) at 0° C., then stirred at 0° C. for a further 60 minutes. The reaction mixture was diluted with acetone (10 ml) then treated with potassium iodide (1.8 g) and copper (I) iodide (2.1 g) and stirred at room temperature for 90 minutes. The reaction mixture was diluted with brine and ethyl acetate then washed with saturated sodium thiosulphate solution. The ethyl acetate layer was separated, dried (MgSO4), filtered and evaporated to give 680 mg of 4-iodo-1H-pyrazole-3-carboxylic acid phenylamide.

出典