HRID1497513

反应详情

EQUATION

反应方程式

HRID 1497513 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a mixture of tert-butyl N-(3-nitrobenzyl)-N-(trifluoroacetyl)glycinate (4.30 g), iron (13.2 g), water (41.8 mL), and ethanol (83.5 mL) was added ammonium chloride (2.54 g) at room temperature, followed by heating and refluxing at 100° C. for 1 hour. After leaving to be cooled, the reaction suspension was filtered through Celite and the filtrate was concentrated under reduced pressure. To the residue was added water, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure to obtain tert-butyl N-(3-aminobenzyl)-N-(trifluoroacetyl)glycinate (3.76 g).

WORKUP

后处理

  1. temperatureby heating
  2. customAfter leaving
  3. temperatureto be cooled
  4. filtrationthe reaction suspension was filtered through Celite
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. additionTo the residue was added water
  7. extractionfollowed by extraction with ethyl acetate
  8. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  9. concentrationconcentrated under reduced pressure