HRID2423244

反应详情

EQUATION

反应方程式

HRID 2423244 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Iron powder (0.78 g) and ammonium chloride (0.15 g) were added in that order to an ethanol/water (4/1) solution (40 mL) of benzyl 2-amino-3-nitrobenzoate (0.38 g), and this was heated under reflux for 20 minutes with vigorous stirring. The insoluble matter was separated by filtration while hot, and the filtrate was evaporated under reduced pressure to about ⅕, and then aqueous sodium hydrogencarbonate solution was added, followed by extraction with ethyl acetate. The organic layer was washed with water, dried, and evaporated under reduced pressure to obtain benzyl 2,3-diaminobenzoate (0.33 g).

WORKUP

后处理

  1. temperaturethis was heated
  2. temperatureunder reflux for 20 minutes with vigorous stirring
  3. customThe insoluble matter was separated by filtration while hot, and the filtrate
  4. customwas evaporated under reduced pressure to about ⅕
  5. additionaqueous sodium hydrogencarbonate solution was added
  6. extractionfollowed by extraction with ethyl acetate
  7. washThe organic layer was washed with water
  8. customdried
  9. customevaporated under reduced pressure