HRID1497513
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureby heating
- customAfter leaving
- temperatureto be cooled
- filtrationthe reaction suspension was filtered through Celite
- concentrationthe filtrate was concentrated under reduced pressure
- additionTo the residue was added water
- extractionfollowed by extraction with ethyl acetate
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure