HRID1762170
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe solution was refluxed for 1 hour
- customThe precipitate was removed by filtration
- concentrationthe filtrate was concentrated in vacuo
- extractionThe residue was extracted with chloroform
- washwashed with saturated sodium chloride solution twice
- dry with materialThe organic solvent layer was dried with anhydrous magnesium sulphate
- concentrationconcentrated in vacuo
- additionn-Hexane was added to the residue
- customcrystallised
- filtrationfollowed by filtration