Реакция #94503

Уравнение реакции

1,2,3-benzenetricarboxylic acid

sulfuric acid

potassium nitrate

→

5-nitro-1,2,3-benzenetricarboxylic acid

Выход 50.4%

Растворители

water

Условия реакции

Обработка

1. 1
   workup.ADDITIONis added, gradually over a 2 hour period
2. 2
   ТемператураThe mixture is heated at 135°-140° C. for 16 hours
3. 3
   Температураcooled
4. 4
   ДругоеSome solid is separated out
5. 5
   workup.DISSOLUTIONis dissolved in water
6. 6
   ЭкстракцияThe entire aqueous mixture is extracted with ether
7. 7
   Промывкаthe extract is washed with water
8. 8
   Сушкаdried over magnesium sulfate
9. 9
   КонцентрированиеThe ether is concentrated to a small volume, and petroleum ether
10. 10
    workup.ADDITIONis added
11. 11
    Другоеto precipitate a white solid
12. 12
    ДругоеThe solid is collected
13. 13
    Другоеdried

Методика

To a stirred mixture of 125 g of 1,2,3-benzenetricarboxylic acid and 900 ml of concentrated sulfuric acid at 60°-70° C. is added, gradually over a 2 hour period, 312 g of potassium nitrate. The mixture is heated at 135°-140° C. for 16 hours, cooled and treated with ice and water. Some solid is separated out and is dissolved in water. The entire aqueous mixture is extracted with ether, the extract is washed with water and dried over magnesium sulfate. The ether is concentrated to a small volume, and petroleum ether is added to precipitate a white solid. The solid is collected and dried to give 76.5 g of 5-nitro-1,2,3-benzenetricarboxylic acid.

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