HRID1822827

反应详情

EQUATION

反应方程式

HRID 1822827 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 1-(Benzyloxy)-2-methoxy-4-nitrobenzene (26 g, 100 mmol) dissolved in ethanol (500 ml) in a 2 liter one-neck flask was added dropwise under 30 minutes a solution af sodium dithionite in water (500 ml), stirring was continued at ambient temperature for 2 h and after that the reaction mixture was heated at 70–80° C. for approx. 4 h, cooled and alkalized with sodium carbonate. The precipitate was filtered, washed with water and dried. The combined water phases were extracted with ethylacetate. The combined organic phases were washed with water, dried over sodium sulfate, filtered and evaporated to dryness. The residue was combined with the filtered precipitate to afford 9.3 g (41% yield) of the product.

WORKUP

后处理

  1. temperatureafter that the reaction mixture was heated at 70–80° C. for approx. 4 h
  2. temperaturecooled
  3. filtrationThe precipitate was filtered
  4. washwashed with water
  5. customdried
  6. extractionThe combined water phases were extracted with ethylacetate
  7. washThe combined organic phases were washed with water
  8. dry with materialdried over sodium sulfate
  9. filtrationfiltered
  10. customevaporated to dryness