HRID551424

反应详情

EQUATION

反应方程式

HRID 551424 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

6-Methyl-1H-indazol-4-amine (75 mg, 0.51 mmol) and iodobenzene (104 mg, 0.51 mmol) were dissolved in DMF (0.55 ml) in a microwave tube. Copper (I) iodide (19 mg, 0.1 mmol), trans-N,N′-dimethyl-1,2-cyclohexanediamine (28.5 mg, 0.2 mmol) and potassium carbonate (140.9 mg, 1.02 mmol) were added and the mixture heated by microwave (250 W) at 100° C. for 20 minutes. The mixture was filtered through a cartridge, washing with DCM (5 ml) and the filtrate was evaporated to dryness and purified by mass-directed autopreparation (system B). The appropriate fractions were combined, extracted with DCM, washed with aqueous sodium bicarbonate, dried through a hydrophobic frit and evaporated to give the title compound (34.9 mg).

WORKUP

后处理

  1. filtrationThe mixture was filtered through a cartridge
  2. washwashing with DCM (5 ml)
  3. customthe filtrate was evaporated to dryness
  4. custompurified by mass-directed autopreparation (system B)
  5. extractionextracted with DCM
  6. washwashed with aqueous sodium bicarbonate
  7. customdried through a hydrophobic frit
  8. customevaporated