HRID1076771

反应详情

EQUATION

反应方程式

HRID 1076771 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8.5 g. of methyl 2-(2-fluoro-2'-nitro-4-biphenylyl)propionate dissolved in 180 ml. of methanol is treated with 36 ml. of 10% aqueous sodium hydroxide solution at reflux temperature for 1 hour. The mixture is concentrated to remove most of the methanol, chilled and acidified with a mixture of 50 ml. of concentrated HCl and 50 g. of ice. The mixture is extracted four times with methylene chloride, the extract washed with water and dried (Na2SO4). Following removal of solvent, the residue crystallizes and is decolorized with activated carbon and crystallized from ether-pentane. 2-(2-fluoro-2'-nitro-4-biphenylyl)propionic acid crystallizes, m.p. 106°-108°.

WORKUP

后处理

  1. concentrationThe mixture is concentrated
  2. customto remove most of the methanol
  3. temperaturechilled
  4. additionacidified with a mixture of 50 ml
  5. extractionThe mixture is extracted four times with methylene chloride
  6. washthe extract washed with water
  7. dry with materialdried (Na2SO4)
  8. customremoval of solvent
  9. customthe residue crystallizes
  10. customcrystallized from ether-pentane
  11. custom2-(2-fluoro-2'-nitro-4-biphenylyl)propionic acid crystallizes