HRID257651

反应详情

EQUATION

反应方程式

HRID 257651 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To the wet product 12 g (~ 0.4 mol) thus obtained, is added methanol (60 ml), water (30 ml), 97% sodium hydroxide (13.0 g) and 9-fluorenone (0.5 g), and glucose (5.5 g) (0.3 mol) is further added to the mixture over an hour while stirring at 50° to 55° C. The mixture is reacted while stirring at 75° C. (boiling point) for 5 hours. As a result, the N-oxide disappears. The reaction liquor is neutralized with 62% sulfuric acid (19.8 g) to pH 8 to precipitate a crystal. The precipitated crystal is separated by filtration, and the separated crystal is fully washed with water and further with methanol. The washed crystal is then dried, thus obtaining 9.4 g of 2-(2'-hydroxy-methylphenyl) benzotriazole having a melting point of 128 to 130° C. at the yield of 92.8%. One can see that the reduction with aromatic ketones takes over 9 hours to complete. This reduction also required the use of two catalysts and a greater amount of total catalysts.

WORKUP

后处理

  1. additionis further added to the mixture over an hour
  2. customThe mixture is reacted
  3. stirringwhile stirring at 75° C. (boiling point) for 5 hours
  4. customto precipitate a crystal
  5. customThe precipitated crystal is separated by filtration
  6. washthe separated crystal is fully washed with water and further with methanol
  7. customThe washed crystal is then dried