HRID1486242

反应详情

EQUATION

反应方程式

HRID 1486242 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

700 mg (1.81 mmol) of ethyl 2,5-dimethyl-7-[(2,3,6-trifluorobenzyl)oxy]pyrazolo[1,5-a]pyridine-3-carboxylate from Example 9A were initially charged in 18 ml of dioxane and heated to 90° C. 4.5 ml of dioxane and 7.25 ml (14.50 mmol) of 2 N aqueous sodium hydroxide solution were added, and the reaction mixture was stirred at 90° C. for two days. Another 3.63 ml (7.26 mmol) of 2 N aqueous sodium hydroxide solution were added and the mixture was stirred at 90° C. for a further 2 hours. The reaction solution was admixed with 15 ml of 1 N aqueous hydrochloric acid and stirred for 30 min. In the course of this, solids precipitated out. This suspension was filtered, and the solids filtered off were washed with a little water and dried under high vacuum. 358 mg of the target compound were obtained (54% of theory).

WORKUP

后处理

  1. stirringthe mixture was stirred at 90° C. for a further 2 hours
  2. stirringstirred for 30 min
  3. customIn the course of this, solids precipitated out
  4. filtrationThis suspension was filtered
  5. filtrationthe solids filtered off
  6. washwere washed with a little water
  7. customdried under high vacuum