反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationThe mixture was filtered through a cartridge
- washwashing with DCM (5 ml)
- customthe filtrate was evaporated to dryness
- custompurified by mass-directed autopreparation (system B)
- extractionextracted with DCM
- washwashed with aqueous sodium bicarbonate
- customdried through a hydrophobic frit
- customevaporated