HRID1269778

反应详情

EQUATION

反应方程式

HRID 1269778 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under a nitrogen atmosphere, 10% Pd—C (1.0 g) was added to a solution of 3-nitro-o-cresol (10.0 g, 65.3 mmol) in methanol (200 ml) at room temperature, and catalytic reduction was carried out at ordinary temperature and atmospheric pressure. After completion of the reaction, the catalyst was filtered off and the filtrate was concentrated under reduced pressure. The resulting residue was dissolved in ethyl acetate, followed by adding thereto acetic anhydride (10.0 ml, 170 mmol) and pyridine (10.6 ml, 131 mmol), and the resulting mixture was refluxed for 2 hours. After completion of the reaction, the reaction mixture was concentrated and hexane was added thereto. The resulting suspension was filtered and the precipitate was dried under reduced pressure to obtain 3-(acetylamino)-2-methylphenyl acetate (12.7 g, 94%).

WORKUP

后处理

  1. customAfter completion of the reaction
  2. filtrationthe catalyst was filtered off
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. dissolutionThe resulting residue was dissolved in ethyl acetate
  5. additionby adding
  6. customAfter completion of the reaction
  7. concentrationthe reaction mixture was concentrated
  8. additionhexane was added
  9. filtrationThe resulting suspension was filtered
  10. customthe precipitate was dried under reduced pressure