HRID53856

反应详情

EQUATION

反应方程式

HRID 53856 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 2,6-di-tert-butyl-4-(2-nitrostyryl)phenol (1.1 g, 3.1 mmol) in methanol (15 ml) was added water (4 ml), conc. hydrochloric acid (0.2 ml) and iron powder (1.7 g, 30 mmol) and the mixture was heated under reflux for 5 hrs. After filtration, followed by extraction with ethyl acetate and water, the extract was washed with water, dried over MgSO4 and concentrated. Purification of the residue by a silica gel column chromatography followed by recrystallization from hexane afforded 4-(2-aminostyryl)-2,6-di-tert-butylphenol (0.70 g, 70%).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 5 hrs
  3. filtrationAfter filtration
  4. extractionfollowed by extraction with ethyl acetate and water
  5. washthe extract was washed with water
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated
  8. customPurification of the residue by a silica gel column chromatography
  9. customfollowed by recrystallization from hexane