HRID34016

反应详情

EQUATION

反应方程式

HRID 34016 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

To a suspension of 544 mg of 6-fluoro-3-[(E)-2-(3-fluorophenyl)-vinyl]-1H-indazole-5-carbonitrile obtained by Example 100 in 2 mL of acetic acid and 3 mL of water was added 6 mL of concentrated sulfuric acid, and stirred at 110° C. for 12 hours. After allowing to cool, the reaction solution was added with ice, and extracted with a mixed solvent of 200 mL of ethyl acetate and 50 mL of tetrahydrofuran. The organic layer was washed successively with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated, to afford 491 mg of the title compound as pale brown crystals.

WORKUP

后处理

  1. temperatureto cool
  2. additionthe reaction solution was added with ice
  3. extractionextracted with a mixed solvent of 200 mL of ethyl acetate and 50 mL of tetrahydrofuran
  4. washThe organic layer was washed successively with water and saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated