HRID660580

反应详情

EQUATION

反应方程式

HRID 660580 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a solution of nitro-(3-oxo-1H,3H-benzo[de]isochromen-1-yl)-acetic acid methyl ester (1.05 g, 3.33 mmol) in EtOH (12 mL) is added acetic acid (4 mL) followed by Fe (560 mg, 10 mmol) and the mixture is stirred at 100° C. for 90 min. Ethyl acetate is added to the mixture and any insoluble material is filtered. The filtrate is washed with water and the organic phase is dried over magnesium sulfate. The solvent is removed under reduced pressure and the residue purified by flash chromatography using a gradient of 0-50% EtOAc/hexane as eluent to give the title compound.

WORKUP

后处理

  1. filtrationany insoluble material is filtered
  2. washThe filtrate is washed with water
  3. dry with materialthe organic phase is dried over magnesium sulfate
  4. customThe solvent is removed under reduced pressure
  5. customthe residue purified by flash chromatography