HRID1684538

反应详情

EQUATION

反应方程式

HRID 1684538 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

230 ml (3.17 mol) of thionyl chloride are run dropwise onto a suspension of 129 g (0.635 mol) of 2-carboxy-6-methoxyquinoline in 1200 ml of toluene, and the mixture is heated for 3 h 30 min. After concentrating the solution under reduced pressure, the solid obtained is dissolved in 300 ml of methanol. The mixture is stirred for 30 min, the solvent is then evaporated off under reduced pressure, and the product obtained is taken up in diethyl ether and isolated by filtration. The solid obtained is taken up in ethyl acetate and dilute aqueous ammonia, and the organic phase is then separated out, treated with animal black, filtered and concentrated under reduced pressure. 90 g of product are thus obtained.

WORKUP

后处理

  1. temperaturethe mixture is heated for 3 h 30 min
  2. concentrationAfter concentrating the solution under reduced pressure
  3. customthe solid obtained
  4. customthe solvent is then evaporated off under reduced pressure
  5. customthe product obtained
  6. customisolated by filtration
  7. customThe solid obtained
  8. customdilute aqueous ammonia, and the organic phase is then separated out
  9. additiontreated with animal black,
  10. filtrationfiltered
  11. concentrationconcentrated under reduced pressure