HRID1270753

反应详情

EQUATION

反应方程式

HRID 1270753 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 2,7-dinitronaphthalene (500 mg, 2.29 mmol) in methanol (5 mL) heated to reflux, is added over 15 minutes, a solution of sodium hydrosulfide (196 mg, 3.44 mmol) in methanol (5 mL) and water (10 mL). The reaction mixture is heated at reflux for 30 minutes and then poured into ice-water and filtered to give an orange solid. After washing the solid with boiling 10% aqueous HCl, the filtrate is basified with solid NaOH and extracted with EtOAc. The organic layer is dried (Na2SO4) and the solvents are evaporated to give 7-nitro-2-aminonaphthalene as a bright orange solid.

WORKUP

后处理

  1. temperatureto reflux
  2. additionis added over 15 minutes
  3. temperatureThe reaction mixture is heated
  4. temperatureat reflux for 30 minutes
  5. filtrationfiltered
  6. customto give an orange solid
  7. washAfter washing the solid
  8. extractionextracted with EtOAc
  9. dry with materialThe organic layer is dried (Na2SO4)
  10. customthe solvents are evaporated