HRID2202443

反应详情

EQUATION

反应方程式

HRID 2202443 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

With the same condition as the method for synthesizing the Compound F5-47 (under nitrogen atmosphere, to the N,N-dimethyl formamide (1.5 ml) solution of 9-bromo-8-(4-cyclobutyl-piperazin-1-yl)-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile (Compound F4-10, 50 mg, 0.099 mmol), trimethyl boroxine (12 mg, 0.1 eq.), tetrakis triphenylphosphine palladium (39 mg, 0.2 eq.), and potassium carbonate (41 mg, 3.0 eq.) were added, and the mixture was stirred at 100° C. for 24 hours. Upon the completion of the reaction, distilled water was poured into the reaction solution, which was then extracted with ethyl acetate. The organic layer was washed with aqueous solution of sodium chloride and dried over sodium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (ethyl acetate/methanol) to obtain the Compound F5-47 (8-(4-cyclobutyl-piperazin-1-yl)-6,6,9-trimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile) (25 mg, 58%)), the title compound was synthesized from the Compound F3-11.

WORKUP

后处理

  1. customWith the same condition as the method for synthesizing the Compound
  2. customUpon the completion of the reaction
  3. distillationdistilled water
  4. additionwas poured into the reaction solution, which
  5. extractionwas then extracted with ethyl acetate
  6. washThe organic layer was washed with aqueous solution of sodium chloride
  7. dry with materialdried over sodium sulfate
  8. customThe drying agent was removed by filtration
  9. customthe residues obtained
  10. concentrationafter concentration under reduced pressure
  11. customwere purified by silica gel column chromatography (ethyl acetate/methanol)
  12. customto obtain the Compound