HRID1854664

反应详情

EQUATION

反应方程式

HRID 1854664 的结构方程式

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a solution of 1H-benzotriazole-5-carboxylic acid (1.00 g, 6.13 mmol) in 30 mL of dry tetrahydrofuran was added lithium aluminum hydride (0.47 g, 12 mmol) under nitrogen at 0° C. After the reaction mixture was stirred at 70° C. for 90 h, saturated Na2SO4 aqueous solution was added carefully at 0° C. After the solution was stirred at room temperature for 30 min, a sufficient amount of Na2SO4 was added with additional stirring for drying. After filtration, the filtrate was concentrated in vacuo, and the residue was purified by silica gel column chromatography (chloroform/methanol=97/3 to 80/20) to obtain (1H-benzoimidazol-5-yl)methanol as a pale yellow solid (143 mg, 16%).

WORKUP

后处理

  1. stirringAfter the solution was stirred at room temperature for 30 min
  2. stirringwith additional stirring
  3. customfor drying
  4. filtrationAfter filtration
  5. concentrationthe filtrate was concentrated in vacuo
  6. customthe residue was purified by silica gel column chromatography (chloroform/methanol=97/3 to 80/20)