反应 #49388

反应方程式

sodium thiosulfate

potassium iodide

urea

sodium nitrate

3-Aminophthalic acid

→

3-iodophthalic acid

收率 62.0%

溶剂

hydrochloric acid

反应条件

后处理

1. 1
   温度cooling for 20 minutes
2. 2
   workup.ADDITIONis added by drops to the mixture
3. 3
   workup.STIRRINGby stirring at room temperature for 20 hours
4. 4
   萃取extracted with ethyl acetate
5. 5
   洗涤The organic layer was washed with saturated brine
6. 6
   干燥dried over anhydrous sodium sulfate
7. 7
   其他The solvent was evaporated under reduced pressure
8. 8
   洗涤the residue was washed with chloroform

实验过程

3-Aminophthalic acid (5.00 g, 27.6 mmol) was dissolved in 8.4 mol/L hydrochloric acid (60 mL), and the solution was added with an aqueous solution (10 mL) of sodium nitrate (2.0 g, 29 mmol) by drops under ice-cooling for 20 minutes, followed by stirring at the same temperature for 3 hours. Then, an aqueous solution (10 mL), in which potassium iodide (6.9 g, 41 mmol) and urea (291 mg) were dissolved, is added by drops to the mixture, followed by stirring at room temperature for 20 hours. The reaction mixture was added with 10% aqueous sodium thiosulfate solution and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was washed with chloroform to obtain 3-iodophthalic acid (5.0 g, yield 62%).

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