HRID245660

反应详情

EQUATION

反应方程式

HRID 245660 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 1-(4-((trans)-4-(8-methylimidazo[1,5-a]pyrazin-3-yl)cyclohexyl)piperazin-1-yl)ethanone (0.422 mmol, 144 mg) in N,N-dimethylformamide (2 mL) was added N-bromosuccinimide (0.422 mmol, 75 mg). After two hours at 60° C. the reaction was quenched with a saturated aqueous sodium hydrogencarbonate solution and extracted twice with ethyl acetate. The organic extracts were washed twice with water and brine, dried (sodium sulfate) and concentrated under reduced pressure. The crude product was purified with column chromatography on silica gel (dichloromethane/methanol) to afford 176 mg of the title compound.

WORKUP

后处理

  1. customAfter two hours at 60° C. the reaction was quenched with a saturated aqueous sodium hydrogencarbonate solution
  2. extractionextracted twice with ethyl acetate
  3. washThe organic extracts were washed twice with water and brine
  4. dry with materialdried (sodium sulfate)
  5. concentrationconcentrated under reduced pressure
  6. customThe crude product was purified with column chromatography on silica gel (dichloromethane/methanol)