HRID2081112

反应详情

EQUATION

反应方程式

HRID 2081112 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
152.5 °C

PROCEDURE

实验过程

A mixture of 2-methyl-5-(5-methyl-[1,3,4]oxadiazol-2-yl)-phenol (0.65 g; 3.42 mmol) (from Example 11 supra) and 4-methoxybenzylamine (3.10 g; 22.6 mmol) (Aldrich) in a sealed reaction vessel was heated in an oil bath at 150-155° C. for 42 hours. The reaction mixture was cooled to room temperature and diluted with dichloromethane and hexanes, forcing the product to precipitate out of solution. The crude solid was collected by filtration and then precipitated again from a dichloromethane-methanol solution as the solvent was evaporated off. The solid was collected and dried, to give 5-[4-(4-methoxy-benzyl)-5-methyl-4H-[1,2,4]triazol-3-yl]-2-methyl-phenol. (Yield 0.849 g, 76.3%).

WORKUP

后处理

  1. customin a sealed reaction vessel
  2. temperatureThe reaction mixture was cooled to room temperature
  3. customto precipitate out of solution
  4. filtrationThe crude solid was collected by filtration
  5. customprecipitated again from a dichloromethane-methanol solution as the solvent
  6. customwas evaporated off
  7. customThe solid was collected
  8. customdried