HRID28621

反应详情

EQUATION

反应方程式

HRID 28621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-(4-amino-phenyl)-malonic acid diethyl ester (450 mg, 1.8 mmol) in anhydrous ether (20 ml), cooled at 0-10° C., was added lithium aluminum hydride (68 mg, 1.8 mmol). After stirring at room temperature for 2 hours, the reaction was cooled to 10° C. and quenched by the addition of hydrated sodium sulfate (2 g). The mixture was filtered and the solid was rinsed with tetrahydrofuran (10 ml). The combined filtrates were concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel eluting with 20% methanol-chloroform to provide 2-(4-amino-phenyl)-propane-1,3-diol (52 mg, 17% yield).

WORKUP

后处理

  1. temperaturethe reaction was cooled to 10° C.
  2. customquenched by the addition of hydrated sodium sulfate (2 g)
  3. filtrationThe mixture was filtered
  4. washthe solid was rinsed with tetrahydrofuran (10 ml)
  5. concentrationThe combined filtrates were concentrated under reduced pressure
  6. customThe residue was purified by flash chromatography on silica gel eluting with 20% methanol-chloroform