HRID239165

反应详情

EQUATION

反应方程式

HRID 239165 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

5 g phenylboronic acid in 30 mL dioxane was added to 3.2 g 3-chloro-5,6,8,9-tetrahydro-1,2,7-triaza-benzocycloheptene-7-carboxylic acid tert-butyl ester and 388 mg (1,1′-bis(diphenyl-phosphinoferrocene)palladium(II)dichloride in 50 mL dioxane under argon. The reaction was stirred at 90° C. over night. The mixture was cooled to RT diluted with water and extracted with ethyl acetate. The organic layer was washed with aqueous sodium hydroxide and brine. The solvent was removed and the precipitate was purified by column chromatographie to yielded 5.5 g of the desired product. (M+H)+=325

WORKUP

后处理

  1. temperatureThe mixture was cooled to RT
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with aqueous sodium hydroxide and brine
  4. customThe solvent was removed
  5. customthe precipitate was purified by column chromatographie