HRID582274

反应详情

EQUATION

反应方程式

HRID 582274 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

5.39 g (18 mmols) of crude 4-(2-hydroxyethyl)-2-[(2-nitrophenyl)azo]phenol synthesized in Example 3 was dissolved in 18 ml of aqueous solution of 2N sodium hydroxide. Subsequently, 9 ml of previously prepared aqueous solution of 25% sodium hydroxide and 5.4 g (83 mmols) of zinc powder were simultaneously added over a period of about 3 hours. The reaction mixture was heated to 70° C. and stirred for about 2 hours. The reaction mixture was then cooled to room temperature and filtered to collect inorganic substance. The obtained mother liquor was acidified with concentrated hydrochloric acid. Precipitated crystals were collected by filtration and recrystalized in toluene, giving 3.70 g of 2-(2H-benzotriazole-2-yl)-4-(2-hydroxyethyl)phenol as yellow crystals (yield 70%, purity 87%).

WORKUP

后处理

  1. temperatureThe reaction mixture was then cooled to room temperature
  2. filtrationfiltered
  3. customto collect inorganic substance
  4. customPrecipitated crystals
  5. filtrationwere collected by filtration
  6. customrecrystalized in toluene