HRID657072

反应详情

EQUATION

反应方程式

HRID 657072 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 6-({[4-(methyloxy)phenyl]methyl}oxy)-3-nitro-2-pyridineamine (4.8 g, 17.5 mmol) and zinc (11 g, 175 mmol) in methanol (200 mL) was added dropwise acetic acid (5 mL) at rt. After 0.5 h the reaction was filtered through celite and then the solvent was evaporated. The residue was partitioned between water (500 mL) and ethyl acetate (500 mL), the phases were separated and the water extracted with ethyl acetate (5×500 mL). The combined organic phases were dried, filtered and evaporated to afford 3.9 g of the title compound as a black solid (91%).

WORKUP

后处理

  1. filtrationAfter 0.5 h the reaction was filtered through celite
  2. customthe solvent was evaporated
  3. customThe residue was partitioned between water (500 mL) and ethyl acetate (500 mL)
  4. customthe phases were separated
  5. extractionthe water extracted with ethyl acetate (5×500 mL)
  6. customThe combined organic phases were dried
  7. filtrationfiltered
  8. customevaporated