HRID1762170

反应详情

EQUATION

反应方程式

HRID 1762170 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-[2-(4-Methoxycarbonylphenoxy)ethyl]phthalimide (158.86 g) prepared in accordance with (1) and 73.33 g of hydrazine hydrate were dissolved in 1.5 liters of methanol and the solution was refluxed for 1 hour. The precipitate was removed by filtration and the filtrate was concentrated in vacuo. The residue was extracted with chloroform and washed with saturated sodium chloride solution twice. The organic solvent layer was dried with anhydrous magnesium sulphate and concentrated in vacuo. n-Hexane was added to the residue to make it crystallised followed by filtration to give 85.74 g of crystals (yield: 90%). M.p. 53°-55.5° C.

WORKUP

后处理

  1. temperaturethe solution was refluxed for 1 hour
  2. customThe precipitate was removed by filtration
  3. concentrationthe filtrate was concentrated in vacuo
  4. extractionThe residue was extracted with chloroform
  5. washwashed with saturated sodium chloride solution twice
  6. dry with materialThe organic solvent layer was dried with anhydrous magnesium sulphate
  7. concentrationconcentrated in vacuo
  8. additionn-Hexane was added to the residue
  9. customcrystallised
  10. filtrationfollowed by filtration