HRID1037524

反应详情

EQUATION

反应方程式

HRID 1037524 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

To a stirred suspension of compound (vi) (3.3 g, 8.6 mmol) in ethanol (35 mL) was added aqueous NaOH (3.44 g, 86 mmol) and the reaction mixture was heated to 90° C. and maintained for 15 h when TLC and LCMS showed the absence of SM and formation of product. Concentration of the solvent gave a crude residue which was dissolved in water and filtered. The filtrate was acidified with dilute HCl at which time the product precipitated and was filtered to give the crude product which was purified by acid-base treatment to give 2-(4-bromophenyl)-5-cyclopropyl-6-nitro-2H-indazole-3-carboxylic acid (vii) (2.2 g, 63%).

WORKUP

后处理

  1. temperaturemaintained for 15 h when TLC and LCMS
  2. customConcentration of the solvent gave a crude residue which
  3. filtrationfiltered
  4. customprecipitated
  5. filtrationwas filtered
  6. customto give the crude product which
  7. customwas purified by acid-base treatment