HRID1729890

反应详情

EQUATION

反应方程式

HRID 1729890 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of fluorene-2-glyoxylic acid (33.7 g) in hydrazine hydrate (50 ml) is refluxed until solution is achieved, cooled and treated with potassium hydroxide (33.7 g) in portions. The mixture is then refluxed for 1 hour, and the excess hydrazine removed by distillation. The residue is dissolved in water and extracted with chloroform. The aqueous layer is acidified to pH 2.0 with 10% HCl and extracted with ether. The ether extracts are washed, dried (MgSO4) and evaporated to give the title compound (29.7 g, mp 184°-186°).

WORKUP

后处理

  1. temperatureis refluxed until solution
  2. temperaturecooled
  3. temperatureThe mixture is then refluxed for 1 hour
  4. customthe excess hydrazine removed by distillation
  5. dissolutionThe residue is dissolved in water
  6. extractionextracted with chloroform
  7. extractionextracted with ether
  8. washThe ether extracts are washed
  9. dry with materialdried (MgSO4)
  10. customevaporated