HRID1809121

反应详情

EQUATION

反应方程式

HRID 1809121 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10.0 g (55 mmol) of 2-hydroxy-3-nitrobenzoic acid was dissolved in 100 mL of ethanol 2 mL of concentrated hydrochloric acid was added dropwise thereto and stirred for 24 hr under heat-reflux. The mixture was cooled to room temperature and concentrated under reduced pressure, followed by dilution with ethyl acetate. The diluted solution was washed with saturated sodium bicarbonate solution and saturated sodium chloride solution, then dried over magnesium sulfate and concentrated under reduced pressure. The resulting residue was subjected to column chromatography (ethyl acetate:hexane=1:4) to obtain the title compound (10.0 g, yield: 86%).

WORKUP

后处理

  1. additionwas added dropwise
  2. temperatureunder heat-reflux
  3. concentrationconcentrated under reduced pressure
  4. washThe diluted solution was washed with saturated sodium bicarbonate solution and saturated sodium chloride solution
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure