HRID2223871

反应详情

EQUATION

反应方程式

HRID 2223871 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N-[2-[1-[2(tert-butyldiphenylsiloxy)ethyl]cyclohexyl]-ethyl]phthalimide (1.52 g) dissolved in ethanol (30 mL) was added hydrazine monohydrate. The reaction solution was heated under reflux for 4 hours. To this was added diethyl ether and the insolbles were filtered off. The solvent was then distilled off under reduced pressure. To this was added chloroform, and the solution was made basic by addition of a 1N aqueous hydroxide solution. The solution was then extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate, filtered, and then, the solvent was distilled off under reduced pressure to give the title compound (1.20 g).

WORKUP

后处理

  1. temperatureThe reaction solution was heated
  2. temperatureunder reflux for 4 hours
  3. filtrationthe insolbles were filtered off
  4. distillationThe solvent was then distilled off under reduced pressure
  5. additionTo this was added chloroform
  6. additionthe solution was made basic by addition of a 1N aqueous hydroxide solution
  7. extractionThe solution was then extracted with chloroform
  8. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  9. filtrationfiltered
  10. distillationthe solvent was distilled off under reduced pressure