HRID1577995

反应详情

EQUATION

反应方程式

HRID 1577995 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 80 ml of a methanol suspension containing 4.31 of N-(2'-methoxycarbonylphenyl)-5,6,7,8tetrahydro-9-oxo-xanthene-2-carboxylic acid amide obtained in Example 43 was added 10 ml of an aqueous solution containing 0.48 g of sodium hydroxide. The mixture was heated for 3 hours under refluxing and stirring conditions. The solvent was then removed by distillation to give a residue which was dissolved in hot water and filtered. The filtrate was acidified with concentrated hydrochloric acid to separate a yellowish white deposit. The deposit was collected by filtration, washed with water and then air-dried. Finally, the deposit was recrystallized from acetic acid to obtain 2.96 g (yield: 71.8%) of N-(2'-carboxyphenyl)-5,6,7,8-tetrahydro-9-oxo-xanthene-2-carboxylic acid amide.

WORKUP

后处理

  1. temperatureThe mixture was heated for 3 hours
  2. temperatureunder refluxing
  3. customThe solvent was then removed by distillation
  4. customto give a residue which
  5. filtrationfiltered
  6. customto separate a yellowish white deposit
  7. filtrationThe deposit was collected by filtration
  8. washwashed with water
  9. customair-dried
  10. customFinally, the deposit was recrystallized from acetic acid