HRID1395284

反应详情

EQUATION

反应方程式

HRID 1395284 的结构方程式

PROCEDURE

实验过程

A mixture of 30 g. of 7-chloro-4-hydroxyquinoline-3-carboxylic acid, ethyl ester, m.p. 299°-301°, (0.12 mol.) and 250 ml. of phosphorus oxychloride is refluxed for 4.5 hours. After removing the excess phosphorus oxychloride, the residue is triturated with water and dissolved in ether. The ethereal solution is washed with aqueous sodium carbonate (5%) and water, dried with sodium sulfate and the solvent is removed. The residual 4,7-dichloroquinoline-3-carboxylic acid, ethyl ester is triturated with petroleum ether (40°-60°), filtered off and dried; yield: 22 g. (68%); m.p. 81°-82°.

WORKUP

后处理

  1. additionA mixture of 30 g
  2. customAfter removing the excess phosphorus oxychloride
  3. customthe residue is triturated with water
  4. dissolutiondissolved in ether
  5. washThe ethereal solution is washed with aqueous sodium carbonate (5%) and water
  6. dry with materialdried with sodium sulfate
  7. customthe solvent is removed
  8. customThe residual 4,7-dichloroquinoline-3-carboxylic acid, ethyl ester is triturated with petroleum ether (40°-60°)
  9. filtrationfiltered off
  10. customdried