HRID7736

反应详情

EQUATION

反应方程式

HRID 7736 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3,5-dimethoxy-N-(2-methoxyphenyl)-4-methylbenzamide (1.29 g, 4.49 mmol), toluene (22 mL), p-toluenesulfonic acid monohydrate (5.9 g, 31 mmol) and molecular sieves was refluxed until no starting material was observed by TLC. Cooled mixture to rt and filtered, washing with warm chloroform. Removal of solvent from filtrate afforded a yellow solid. Purification of crude solid by flash chromatography on silica gel using 1:3 EtOAc:hexanes gave the desired intermediate, 2-(3,5-dimethoxy-4-methylphenyl)-1,3-benzoxazole, as a colorless solid.

WORKUP

后处理

  1. temperaturewas refluxed until no starting material
  2. filtrationfiltered
  3. washwashing with warm chloroform
  4. customRemoval of solvent from filtrate
  5. customafforded a yellow solid
  6. customPurification of crude solid by flash chromatography on silica gel using 1:3 EtOAc