HRID1468302

反应详情

EQUATION

反应方程式

HRID 1468302 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

7-Bromo-2-isopropylimidazo[1,2-a]pyridine (1.00 g, 4.18 mmol) obtained in step 1 of Example 28 was dissolved in 1,2-dichloroethane (10 mL). Under ice-cooled condition, trimethylsilyl chlorosulfonate (1.20 mL, 8.36 mmol) was added, and the mixture was stirred at 90° C. for 3 hours. Under ice-cooled condition, triethylamine (1.17 mL, 8.36 mmol) and phosphoryl chloride (0.779 mL, 8.36 mmol) were added, and the mixture was stirred at 100° C. for 1.5 hours. The solvent was evaporated under reduced pressure, and the residue was dissolved in acetonitrile. After adding a sodium hydrogen carbonate aqueous solution, the precipitated solid was collected by filteration to give 7-bromo-2-isopropylimidazo[1,2-a]pyridine-3-sulfonylchloride (1.31 g, yield 93%).

WORKUP

后处理

  1. additionwas added
  2. additionwere added
  3. stirringthe mixture was stirred at 100° C. for 1.5 hours
  4. customThe solvent was evaporated under reduced pressure
  5. dissolutionthe residue was dissolved in acetonitrile
  6. additionAfter adding a sodium hydrogen carbonate aqueous solution
  7. customthe precipitated solid was collected by filteration