HRID1878461

反应详情

EQUATION

反应方程式

HRID 1878461 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

To a solution of 852 μL of aniline in 104 mL of toluene cooled to 0° C. are added dropwise 6.2 mL of a 2M solution of trimethylaluminium in toluene, followed by addition, at 20° C., of 1.5 g of ethyl 6-iodo-5-methyl(pyrid-2-yl)imidazo[1,2-a]pyridine-2-carboxylate. The reaction mixture is stirred for 2 hours at 20° C. The resulting mixture is cooled to 4° C. and 120 mL of saturated ammonium chloride solution are then added. After concentrating under reduced pressure, the residue is taken up in ethyl acetate and the organic phase is washed with water, dried over magnesium sulfate, filtered through Celite and evaporated to dryness under reduced pressure. The residue is triturated in methanol, filtered off and dried to give 1.15 g of 6-iodo-5-methyl-N-phenyl(pyrid-2-yl)imidazo[1,2-a]pyridine-2-carboxamide in the form of a yellow solid.

WORKUP

后处理

  1. temperatureThe resulting mixture is cooled to 4° C.
  2. concentrationAfter concentrating under reduced pressure
  3. washthe organic phase is washed with water
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered through Celite
  6. customevaporated to dryness under reduced pressure
  7. customThe residue is triturated in methanol
  8. filtrationfiltered off
  9. customdried