HRID1458737

反应详情

EQUATION

反应方程式

HRID 1458737 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

K2CO3 (13.94 g, 0.101 mol) is dissolved in water (67 ml), and then 2-iodo-4-methoxybenzoic acid (25.3 g, 0.091 mol) is added, followed by 5-amino-1-ethylpyrazole (11.2 g, 0.101 mol) and finally copper (2.7 g). The reaction mixture is refluxed for 20 hours, cooled to room temperature. Then water (350 ml) is added, and the mixture is refluxed for 0.75 hours. The reaction mixture is cooled, and the product is collected by filtration, recrystallized from ethanol, and dried in an oven at 40° C. to afford 13.37 g (56%) of N-(1-ethylpyrazol-5-yl)-4-methoxyanthranilic acid, m.p. 130°-135° C.

WORKUP

后处理

  1. temperatureThe reaction mixture is refluxed for 20 hours
  2. temperaturethe mixture is refluxed for 0.75 hours
  3. temperatureThe reaction mixture is cooled
  4. filtrationthe product is collected by filtration
  5. customrecrystallized from ethanol
  6. customdried in an oven at 40° C.