HRID270124

反应详情

EQUATION

反应方程式

HRID 270124 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

A solution of methyl 3-hydroxy-4-nitrobenzoate (0.78 g, 3.96 mmol) in THF (40 ml) with Pd on charcoal (10%, 0.15 g) was stirred in the atmosphere of hydrogen at atmospheric pressure overnight. The mixture was filtered through celite. The solvent was removed in vacuo. The residue was taken into water (20 ml), and acetic anhydride (0.5 ml, 5.29 mmol) was added. The mixture was vigorously stirred at 65° C. for 30 min. After cooling to room temperature, the precipitate was collected by filtration, washed with water, and dried. White powder (0.64 g, 77%).

WORKUP

后处理

  1. filtrationThe mixture was filtered through celite
  2. customThe solvent was removed in vacuo
  3. additionwas added
  4. temperatureAfter cooling to room temperature
  5. filtrationthe precipitate was collected by filtration
  6. washwashed with water
  7. customdried