HRID2075720

反应详情

EQUATION

反应方程式

HRID 2075720 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

7-Iodo-1-phenyl-[1,2,4]triazolo[4,3-a]quinoline (10c, 140 mg, 0.38 mmol), copper iodide (14 mg, 0.08 mmol), and potassium carbonate (105 mg, 0.76 mmol) were suspended in iPrOH (1 mL). 10b (92 mg, 0.38 mmol) in iPrOH (1 mL) was added, followed by ethyl glycol (0.04 mL, 0.76 mmol), and the reaction was heated to 90° C. overnight. The reaction was diluted with EtOAc and water, and the aqueous layer was extracted with EtOAc. The combined organic layers were dried over MgSO4, filtered, and concentrated. The residue was purified by silica gel chromatography (5% MeOH in CH2Cl2), and the isolated product was precipitated from CH2Cl2 to give the desired product, 10d.

WORKUP

后处理

  1. extractionthe aqueous layer was extracted with EtOAc
  2. dry with materialThe combined organic layers were dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel chromatography (5% MeOH in CH2Cl2)
  6. customthe isolated product was precipitated from CH2Cl2