HRID1972229

反应详情

EQUATION

反应方程式

HRID 1972229 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A reaction tube charged with 1-(4-(4-chlorophenoxy)phenyl)-5-(3-(trifluoromethyl)phenyl)imidazolidin-2-one (20.0 mg, 0.0462 mmol), 4-iodoanisole (13.0 mg, 0.0554 mmol), K3PO4 (19.6 mg, 0.0924 mmol), and catalytic amount of CuI is purged with nitrogen. 1,4-Dioxane (0.5 mL) and catalytic amount of trans-1,2-diaminocyclohexane are added via syringe. The reaction mixture is heated at 100° C. overnight, cooled down to room temperature, quenched with saturated NH4Cl aqueous solution (5 mL), and extracted with EtOAc (3×3 mL). The combined organic layer is concentrated and purified by preparatory LC/MS to provide the title compound; HPLC-MS calculated for C29H22ClF3N2O3 (M+H+) 539.1, found 539.1.

WORKUP

后处理

  1. customis purged with nitrogen
  2. addition1,4-Dioxane (0.5 mL) and catalytic amount of trans-1,2-diaminocyclohexane are added via syringe
  3. temperaturecooled down to room temperature
  4. customquenched with saturated NH4Cl aqueous solution (5 mL)
  5. extractionextracted with EtOAc (3×3 mL)
  6. concentrationThe combined organic layer is concentrated
  7. custompurified by preparatory LC/MS