HRID276972

反应详情

EQUATION

反应方程式

HRID 276972 的结构方程式

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 9 ml of salicylaldehyde (84.46 mmol), 17 ml of aqueous 37% formaldehyde solution (˜200 mmol) and 42 ml of concentrated HCl is heated on a water bath at 80° C. with stirring for 20 min. After cooling, the supernatant is removed by settling of the phases and the residual pink crystalline mass is taken up in 200 ml of boiling water. The suspension obtained is refluxed for 30 min. The supernatant is separated out after settling and placed at +4° C. to bring about crystallization of the final product. A further 200 ml of boiling water are added to the residual oil and the suspension is refluxed for 30 min. The supernatant is added to the first decantate. After cooling, the product is collected by filtration, washed with water and dried. It is then recrystallized from chloroform.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe supernatant is removed
  3. customThe suspension obtained
  4. temperatureis refluxed for 30 min
  5. customThe supernatant is separated out
  6. customplaced at +4° C.
  7. customto bring about crystallization of the final product
  8. additionA further 200 ml of boiling water are added to the residual oil
  9. temperaturethe suspension is refluxed for 30 min
  10. additionThe supernatant is added to the first decantate
  11. temperatureAfter cooling
  12. filtrationthe product is collected by filtration
  13. washwashed with water
  14. customdried
  15. customIt is then recrystallized from chloroform