HRID1846947

反应详情

EQUATION

反应方程式

HRID 1846947 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a round bottom flask was added ethyl-5-bromo-2-(trifluoromethoxy)benzoate (0.638 mmole) in ethanol (10 mL). To this solution was added 1 mL of hydrazine monohydrate and the resulting mixture was refluxed overnight. The reaction mixture was evaporated in vacuo to give A. To A was added trimethylorthoformate in a heavy wall pressure tube. This resulting mixture was heated at 100 C for 18 hours. The reaction mixture was concentrated down and purified by preparative TLC to afford B which was coupled with 3-(trifluoromethyl)-[1,2,4]triazolo[4,3-a]pyridin-6-ylboronic acid using methods disclosed above to give 2-(2-(trifluoromethoxy)-5-(3-(trifluoromethyl)-[1,2,4]triazolo[4,3-a]pyridin-6-yl)phenyl)-1,3,4-oxadiazole.

WORKUP

后处理

  1. temperaturethe resulting mixture was refluxed overnight
  2. customThe reaction mixture was evaporated in vacuo
  3. customto give A
  4. temperatureThis resulting mixture was heated at 100 C for 18 hours
  5. concentrationThe reaction mixture was concentrated down
  6. custompurified by preparative TLC
  7. customto afford B which