HRID1045090

反应详情

EQUATION

反应方程式

HRID 1045090 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The fluorenone imine (1.52 g, 8.48 mmol) and the glycine tert-butylester hydrochloride (1.42 g, 8.48 mmol) were stirred in the methylene chloride for five hours at room temperature. The reaction solution was filtered with celite, and the solvent was removed by the distillation under reduced pressure. The obtained residual was allowed to dissolve in the diethyl ether. And, it was filtered with the celite. The obtained ether solution was cleaned with water and a saturated sodium chloride aqueous solution. And, it was dried over sodium sulfate. After the filtering and the concentration under reduced pressure were conducted, the obtained crude product was refined with the diethyl ether/hexane (recrystallization). And, (Fluoren-9-ylideneamino)-acetic acid tert-butyl ester (1.18 g, 66%) was obtained.

WORKUP

后处理

  1. filtrationThe reaction solution was filtered with celite
  2. customthe solvent was removed by the distillation under reduced pressure
  3. dissolutionto dissolve in the diethyl ether
  4. filtrationAnd, it was filtered with the celite
  5. dry with materialAnd, it was dried over sodium sulfate
  6. concentrationAfter the filtering and the concentration under reduced pressure
  7. customthe obtained crude product