HRID2091006

反应详情

EQUATION

反应方程式

HRID 2091006 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of methyl 4-{[3-methyl-1-(3-methyl-1-benzofuran-2-yl)butyl]amino}benzoate (1.38 g) synthesized above, tetrahydrofuran (20 mL) and ethanol (20 mL) was added 1N aqueous sodium hydroxide solution (20 mL), and the mixture was stirred with heating under reflux overnight. In addition, 1N aqueous sodium hydroxide solution (20 mL) was added, and the mixture was stirred with heating under reflux for 3 hr. The reaction mixture was concentrated under reduced pressure, 1N hydrochloric acid (40 mL) was added to the residue, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was washed with diisopropyl ether to give the title object compound (1.06 g, 80%) as a white solid.

WORKUP

后处理

  1. temperaturewith heating
  2. temperatureunder reflux overnight
  3. stirringthe mixture was stirred
  4. temperaturewith heating
  5. temperatureunder reflux for 3 hr
  6. concentrationThe reaction mixture was concentrated under reduced pressure, 1N hydrochloric acid (40 mL)
  7. additionwas added to the residue
  8. extractionthe mixture was extracted with ethyl acetate
  9. washThe extract was washed with water and saturated brine
  10. dry with materialdried over magnesium sulfate
  11. concentrationconcentrated under reduced pressure
  12. washThe residue was washed with diisopropyl ether