HRID368734

反应详情

EQUATION

反应方程式

HRID 368734 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

700 mmol of dimethyl succinate and then 20 ml of methanol are added to 290 mmol of sodium methylate dissolved in 80 ml of methanol. The mixture is brought to reflux, and 236 mmol of benzaldehyde are slowly added, followed by 20 ml of methanol. The mixture is maintained at reflux, with stirring, for one hour, and then 100 ml of methanol are distilled off. 120 ml of water and 120 ml of 10N sodium hydroxide solution are added to the concentrated reaction mixture. The removal of the methanol by distillation is continued. The residue is diluted with 150 ml of water. After the addition of dichloromethane, the diacid is precipitated by the slow addition of 12N hydrochloric acid. The diacid is filtered and washed with dicliloromethane and then with water. Drying yields the expected product.

WORKUP

后处理

  1. temperatureto reflux
  2. temperatureThe mixture is maintained
  3. temperatureat reflux
  4. distillation100 ml of methanol are distilled off
  5. addition120 ml of water and 120 ml of 10N sodium hydroxide solution are added to the concentrated reaction mixture
  6. customThe removal of the methanol
  7. distillationby distillation
  8. additionThe residue is diluted with 150 ml of water
  9. additionAfter the addition of dichloromethane
  10. customthe diacid is precipitated by the slow addition of 12N hydrochloric acid
  11. filtrationThe diacid is filtered
  12. washwashed with dicliloromethane
  13. customDrying