HRID84771

反应详情

EQUATION

反应方程式

HRID 84771 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

1.7 g tetrakis was added to a stirred mixture of 15 g 1-(4-pyrimidin-2-yl-piperazin-1-yl)-2-(2, 4, 5-tribromo-imidazol-1-yl)-ethanone, 3.6 g phenylboronic acid, 9.4 g sodiumcarbonate, 250 mL dioxane and 50 mL water under nitrogen atmosphere. The reaction mixture was stirred 3 h at 85° C. Sodium hydrogen carbonate solution was added and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride solution, dried over sodium sulfate and evaporated. Diisopropylether was added to the residue and the precipitate was filtered to give 11.8 g desired product. Rt: 0.87 (method B), ESI+: 505

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with saturated sodium chloride solution
  3. dry with materialdried over sodium sulfate
  4. customevaporated
  5. additionDiisopropylether was added to the residue
  6. filtrationthe precipitate was filtered