HRID1446661

反应详情

EQUATION

反应方程式

HRID 1446661 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Treat a solution of 7-(4-methanesulfonyl-phenyl)-imidazo[1,2-a]pyridine (101 g, 371.3 mmol, 1 eq) in 2000 mL of CH3CN at 0° C. with NIS (83.5 g, 371.3 mmol, 1 eq). Allow the mixture to stir at room temperature for 1 hour. Remove the solvent and the dissolve the residue in 5000 mL of CH2Cl2, wash with 10% NaOH solution, NaHSO3 sat., water and aqueous saturated sodium chloride. Dry over MgSO4 and evaporate. Triturate the solid obtained with hexanes, filter and dry in vacuo to afford 110 g of the title compound as a yellow solid. (Yield: 75%). MS (ES), m/z 399 (M+1).

WORKUP

后处理

  1. customRemove the solvent
  2. dissolutionthe dissolve the residue in 5000 mL of CH2Cl2
  3. washwash with 10% NaOH solution, NaHSO3 sat., water and aqueous saturated sodium chloride
  4. dry with materialDry over MgSO4
  5. customevaporate
  6. customTriturate the solid
  7. customobtained with hexanes
  8. filtrationfilter
  9. customdry in vacuo