HRID523952

反应详情

EQUATION

反应方程式

HRID 523952 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a stirred solution of H2O (80 mL) and H2SO4 (120 mL) at 0° C. was added 5-bromo-8-methylquinoline (25 g, 112.6 mmol). After obtaining a solution, CrO3 was introduced (16 g, 157.6 mmol) in portion wise while maintaining the internal temperature at 70° C. The reaction mixture was stirred for 1 h at 70° C. An additional CrO3 (16 g, 157.6 mmol) was added in portions and stirred at 80° C. for 2.5 h. After completion of the reaction, it was cooled to r.t, poured onto crushed ice, neutralized with aqueous ammonium hydroxide to get the solids. The solids were filtered, dried under high vacuum for 16 h to get the crude 5-bromoquinoline-8-carboxylic acid (28.0 g) as a green colored solid.

WORKUP

后处理

  1. customAfter obtaining a solution, CrO3
  2. additionwas introduced (16 g, 157.6 mmol) in portion wise
  3. stirringstirred at 80° C. for 2.5 h
  4. customAfter completion of the reaction, it
  5. temperaturewas cooled
  6. additionpoured
  7. customonto crushed ice
  8. customto get the solids
  9. filtrationThe solids were filtered
  10. customdried under high vacuum for 16 h