HRID2109940
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
- 150 °C
PROCEDURE
实验过程
A mixture of 2-chloronicotinamide (59 mg, 0.37 mmol), potassium carbonate (57 mg, 0.41 mmol), 3-(4-fluorophenyl)-1-(2-methylphenyl)-1H-pyrazol-5-amine (100 mg, 0.37 mmol) (Intermediate G), and copper (II) acetate (1.4 mg, 0.007 mmol) in DMF (1 mL) was heated (150° C.) in a sealed tube for 16 h. The mixture was cooled to rt, filtered through a silica gel plug using ethyl acetate as eluent, concentrated to dryness, and subjected to HPLC purification using a gradient elution from 30% to 90% acetonitrile in water to afford 20 mg (14%) of the desired product.
WORKUP
后处理
- temperatureThe mixture was cooled to rt
- filtrationfiltered through a silica gel plug
- concentrationconcentrated to dryness
- customsubjected to HPLC purification
- washa gradient elution from 30% to 90% acetonitrile in water