反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customAfter obtaining a solution, CrO3
- additionwas introduced (16 g, 157.6 mmol) in portion wise
- stirringstirred at 80° C. for 2.5 h
- customAfter completion of the reaction, it
- temperaturewas cooled
- additionpoured
- customonto crushed ice
- customto get the solids
- filtrationThe solids were filtered
- customdried under high vacuum for 16 h