HRID1179655

反应详情

EQUATION

反应方程式

HRID 1179655 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

5-{4-[2-(3-Iodophenyl)ethyl]-1-piperazinyl}-2-methylquinoline (59 mg), 5,6-dihydro-1H-imidazo[2,1-c][1,2,4]triazole (50 mg, 3.5 equiv.), palladium(II)acetate (9 mg, 0.3 equiv.) 2-(dicyclohexylphosphino)-2′-methylbiphenyl (42 mg, 0.9 equiv.) and potassium phosphate (97 mg, 3.5 equiv.) were suspended in DME and stirred at 150 □C under microwave irradiation for 2 h. The mixture was cooled to room temperature, diluted with methanol and loaded onto an ion-exchange cartridge (SCX-2), which was eluted with methanol followed by ammonia-methanol solution (1M). The combined basic fractions were concentrated under vacuum and purified using column chromatography [SiO2; DCM-MeOH (90:10)] to afford the title compound as colourless solid (13 mg, 26% yield).

WORKUP

后处理

  1. washwas eluted with methanol
  2. concentrationThe combined basic fractions were concentrated under vacuum
  3. custompurified