HRID1588064

反应详情

EQUATION

反应方程式

HRID 1588064 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3-Methyl-6-nitroindazole (5.31 g), 6.93 g of 2-bromo-6-methoxybenzoic acid, 4.71 g of potassium carbonate and 0.218 g of copper (II) oxide were stirred in 60 ml of nitrobenzene at 180° C. for 50 minutes. After cooling, 300 ml of water was added to the reaction mixture, and the insoluble substance was removed by filtration. The resulting solution was washed with chloroform. The aqueous layer was decolored with active charcoal and filtered, and 40 ml of 1 N hydrochloric acid aqueous solution was added to the filtrate. The crystals precipitated were separated by filtration and dried under reduced pressure to obtain 7.45 g (75.9%) of 1-(2-carboxy-3-methoxyphenyl)-3-methyl-6-nitroindazole.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe insoluble substance was removed by filtration
  3. washThe resulting solution was washed with chloroform
  4. filtrationfiltered
  5. addition40 ml of 1 N hydrochloric acid aqueous solution was added to the filtrate
  6. customThe crystals precipitated
  7. customwere separated by filtration
  8. customdried under reduced pressure