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
- 0 °C
PROCEDURE
实验过程
6-Methylisoquinoline (46.3 g, 0.323 mol) obtained in Step (1) was mixed with sulfuric acid (400 mL) and stirred. The temperature of the reaction solution was cooled to 0° C. or lower, slowly added with potassium nitrate (65.3 g, 0.646 mol) and stirred for 3 hours or more at 0° C. The reaction mixture was added with an ice water, and adjusted to have a pH value of 12 by adding 5N aqueous NaOH solution, followed by stirring for 12 hours or more at room temperature. The solid thus obtained was filtered under reduced pressure, and the resulting solid was washed with water. The filtered solid was dried with warm wind in an oven (40° C.) for 3 hours or more to obtain the title compound (43.3 g, 71%).
WORKUP
后处理
- stirringstirred for 3 hours or more at 0° C
- stirringby stirring for 12 hours or more at room temperature
- customThe solid thus obtained
- filtrationwas filtered under reduced pressure
- washthe resulting solid was washed with water
- customThe filtered solid was dried
- temperaturewith warm wind in an oven (40° C.) for 3 hours or more