HRID250757

反应详情

EQUATION

反应方程式

HRID 250757 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

Add dioxane (7 mL) to a mixture of 3-phenyl-1H-pyrazole (2 g, 13.9 mmol), copper iodide (132 mg, 0.05 mmol) and potassium carbonate (555 mg, 4.2 mmol). Add 2-fluoroiodobenzene (1.94 mL, 16.6 mmol), trans-cyclohexyldiamine (0.35 mL, 2.78 mmol). Heat at 110° C. for about 18 hours. Cool to RT and filter through a silica gel pad eluting with ethyl acetate. Concentrate and purify (silica gel chromatography, eluting with hexane:ethyl acetate 84:16) to give the desired compound (36%).

WORKUP

后处理

  1. temperatureCool to RT
  2. filtrationfilter through a silica gel pad
  3. washeluting with ethyl acetate
  4. concentrationConcentrate
  5. custompurify
  6. wash(silica gel chromatography, eluting with hexane:ethyl acetate 84:16)