HRID371798

反应详情

EQUATION

反应方程式

HRID 371798 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. additionis added, gradually over a 2 hour period
  2. temperatureThe mixture is heated at 135°-140° C for 16 hours
  3. temperaturecooled
  4. customSome solid is separated out
  5. dissolutionis dissolved in water
  6. extractionThe entire aqueous mixture is extracted with ether
  7. washthe extract is washed with water
  8. dry with materialdried over magnesium sulfate
  9. concentrationThe ether is concentrated to a small volume, and petroleum ether
  10. additionis added
  11. customto precipitate a white solid
  12. customThe solid is collected
  13. customdried