HRID613271

反应详情

EQUATION

反应方程式

HRID 613271 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) was dissolved in water (67 ml) and then 2-iodo-4-methoxybenzoic acid (25.3 g, 0.091 mol) was added, followed by 5-amino-1-ethylpyrazole (11.2 g, 0.101 mol) and finally copper (2.7 g). The reaction mixture was refluxed for 20 hours, cooled to room temperature and then water (350 ml) was added and the mixture was refluxed for 0.75 hours. The reaction mixture was cooled, and the product was 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 was refluxed for 20 hours
  2. temperaturethe mixture was refluxed for 0.75 hours
  3. temperatureThe reaction mixture was cooled
  4. filtrationthe product was collected by filtration
  5. customrecrystallized from ethanol
  6. customdried in an oven at 40° C.