HRID1096998

反应详情

EQUATION

反应方程式

HRID 1096998 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 3.0-liter egg plant type flask, iodine (6.09 g, 24 mmol) and KOH (4.49 g, 68 mmol) were added to a DMF solution (60 mL) of ethyl 1H-indazole-6-carboxylate (4.52 g, 20 mmol), and stirred at room temperature for 2 hours. Saturated ammonium chloride water was added to it, extracted with ethyl acetate, washed with water and saturated saline water in that order, and dried with sodium sulfate. The reaction solution was filtered, concentrated, and the resulting solid was washed with a mixed solution of hexane and ethyl acetate to obtain the title compound as a yellow solid.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washwashed with water and saturated saline water in that order
  3. dry with materialdried with sodium sulfate
  4. filtrationThe reaction solution was filtered
  5. concentrationconcentrated
  6. washthe resulting solid was washed with a mixed solution of hexane and ethyl acetate