HRID418769

反应详情

EQUATION

反应方程式

HRID 418769 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

1H-Indazol-4-amine (81 mg, 0.61 mmol) and methyl 3-iodobenzoate (160 mg, 0.61 mmol) were dissolved in DMF (1 mL) in a microwave tube. Copper (I) iodide (23 mg, 0.12 mmol), trans-N,N′-dimethyl-1,2-cyclohexanediamine (34 mg, 0.24 mmol) and potassium carbonate (169 mg, 1.22 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. The appropriate fractions were evaporated, dissolved in DCM (10 mL), washed with aqueous sodium bicarbonate, and evaporated to give the title compound (32.7 mg).

WORKUP

后处理

  1. filtrationThe mixture was filtered through a cartridge
  2. washwashing with DCM (5 mL)
  3. customthe filtrate was evaporated to dryness
  4. custompurified by mass-directed autopreparation
  5. customThe appropriate fractions were evaporated
  6. dissolutiondissolved in DCM (10 mL)
  7. washwashed with aqueous sodium bicarbonate
  8. customevaporated