HRID328975

反应详情

EQUATION

反应方程式

HRID 328975 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a hot stirred solution of 20.5 g. (134 mM) of phthalaldehydic acid and 17.95 g. (135 mM) of rhodanine in 90 ml. of glacial acetic acid is added 36.0 g. (438 mM) of sodium acetate. While heating the resulting solution to reflux, a precipitate forms and an additional 30 ml. of acetic acid is added. After refluxing the mixture for 0.5 hour, it is cooled, poured into water, and filtered to separate a yellow solid. The solid is washed with water and boiled with 500 ml. of isopropanol. The resulting mixture is cooled and filtered to separate 31.14 g. (87.5%) of the 5-o-carboxybenzylidenerhodanine as yellow needles, m.p. 276°-278°.

WORKUP

后处理

  1. temperatureWhile heating the resulting solution
  2. temperatureto reflux
  3. temperatureAfter refluxing the mixture for 0.5 hour
  4. temperatureit is cooled
  5. filtrationfiltered
  6. customto separate a yellow solid
  7. washThe solid is washed with water
  8. temperatureThe resulting mixture is cooled
  9. filtrationfiltered
  10. customto separate 31.14 g