HRID1727110

反应详情

EQUATION

反应方程式

HRID 1727110 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Iodine (1.53 g, 6.02 mmol) and potassium hydroxide pellets (805 mg, 14.3 mmol) were added successively into a DMF solution of 6-(2-Fluoro-phenoxy)-1H-indazole (1.35 g, 5.92 mmol) at room temperature under stirring. After 1.5 h the reaction was poured into sodium bisulfite solution and extracted into EtOAc (2×20 mL). The combined organic layers were dried over Na2SO4 filtered, concentrated and the residue was purified by flash chromatography eluting with Hex:EtOAc 9:1 to yield 1.9 g of 6-(2-fluoro-phenoxy)-3-iodo-1H-indazole: MS: 355 (M+H).

WORKUP

后处理

  1. extractionextracted into EtOAc (2×20 mL)
  2. dry with materialThe combined organic layers were dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customthe residue was purified by flash chromatography
  6. washeluting with Hex