HRID128543

反应详情

EQUATION

反应方程式

HRID 128543 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-fluoro-4-chloro-5-hydroxynitrobenzene (7.1 g, 37.1 mmol) and potassium carbonate (5.1 g, 37.1 mmol) in acetonitrile (300 ml) was stirred for 2 hours at a refluxing temperature. Cyclopentyl p-toluenesulfonate (10.3 g, 40.8 mmol) was added thereto, followed by stirring further for 2 hours under refluxing. After completion of the reaction, the solvent was distilled off under reduced pressure from the reaction mixture, 1N hydrochloric acid (800 ml) was added thereto, and the mixture was extracted with ethyl acetate (100 ml×3 times). The organic layer was washed with an aqueous solution of sodium bicarbonate and water, dried, and the solvent was distilled off under reduced pressure to obtain 2-fluoro-4-chloro-5-cyclopentyloxynitrobenzene as a yellow solid (8.93 g, 34.3 mmol, 92.6% yield).

WORKUP

后处理

  1. temperatureunder refluxing
  2. customAfter completion of the reaction
  3. distillationthe solvent was distilled off under reduced pressure from the reaction mixture, 1N hydrochloric acid (800 ml)
  4. additionwas added
  5. extractionthe mixture was extracted with ethyl acetate (100 ml×3 times)
  6. washThe organic layer was washed with an aqueous solution of sodium bicarbonate and water
  7. customdried
  8. distillationthe solvent was distilled off under reduced pressure