HRID2233040

反应详情

EQUATION

反应方程式

HRID 2233040 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A suspension of 440 mg of 2,6-di-tert-butyl-8-chloro-5-o-tolyl-2H-[1,2,4]triazolo[4,3-a]pyrazin-3-one and 504 mg of aluminum trichloride in dichloroethane (12.0 mL) was heated to 100° C. After one h, the reaction was cooled to ambient temperature and the excess aluminum reagent was quenched by the careful addition of water. This mixture was diluted with chloroform and the layers were separated. The organic layer was washed with water and then sat. sodium chloride solution, dried over sodium sulfate, filtered, and concentrated. The residue was purified by silica gel chromatography to afford 6-tert-butyl-8-chloro-5-o-tolyl-2H-[1,2,4]triazolo[4,3-a]pyrazin-3-one as a yellow solid. MS (M+H−)=315.1.

WORKUP

后处理

  1. temperatureAfter one h, the reaction was cooled to ambient temperature
  2. customthe excess aluminum reagent was quenched by the careful addition of water
  3. additionThis mixture was diluted with chloroform
  4. customthe layers were separated
  5. washThe organic layer was washed with water
  6. dry with materialsat. sodium chloride solution, dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe residue was purified by silica gel chromatography