HRID18542

反应详情

EQUATION

反应方程式

HRID 18542 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1 g 2-(2-Methoxy-ethoxy)-6-nitro-phenylamine in 10 mL ethyl acetate and 3 mL ethanol, 4.4 g SnCl2 dihydrate were added and the reaction mixture was heated to reflux for 6 h. Then, after cooling 50 mL 2 M NaOH were added and the inorganic precipitate was filtered and washed extensivley with ethyl acetate. The filtrate was extracted with exthyl acetate (3×100 ml), the combined organic layers were dried over MgSO4, and the solvents were removed under reduced pressure. The remaining product was pure enough for the next reaction step.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureto reflux for 6 h
  3. additionwere added
  4. filtrationthe inorganic precipitate was filtered
  5. washwashed extensivley with ethyl acetate
  6. extractionThe filtrate was extracted with exthyl acetate (3×100 ml)
  7. dry with materialthe combined organic layers were dried over MgSO4
  8. customthe solvents were removed under reduced pressure
  9. customThe remaining product was pure enough for the next reaction step