反应 #9561

反应方程式

Butyryl chloride

7-bromo-N4-(2-methylpropyl)quinoline-3,4-diamine

→

7-bromo-1-(2-methylpropyl)-2-propyl-1H-imidazo[4,5-c]quinoline

溶剂

pyridine

反应条件

后处理

1. 1
   其他A pale yellow precipitate formed
2. 2
   温度The reaction mixture was heated
3. 3
   温度at reflux for eight hours
4. 4
   浓缩was concentrated under reduced pressure
5. 5
   workup.DISSOLUTIONThe residue was dissolved in 1 N hydrochloric acid
6. 6
   workup.ADDITIONadjusted to pH 14 with the addition of 10% aqueous sodium hydroxide
7. 7
   其他A precipitate formed
8. 8
   其他was isolated by filtration
9. 9
   洗涤washed with water (3×100 mL)
10. 10
    其他dried overnight on the filter funnel

实验过程

Butyryl chloride (1.1 equivalent) was slowly added to a stirred solution of 7-bromo-N4-(2-methylpropyl)quinoline-3,4-diamine (52.9 g, 0.18 mol.) in pyridine (700 mL) at room temperature. A pale yellow precipitate formed and then went into solution. The reaction mixture was heated at reflux for eight hours, and then allowed to slowly cool to room temperature over the weekend. The dark gold, turbid reaction mixture was concentrated under reduced pressure. The residue was dissolved in 1 N hydrochloric acid and then adjusted to pH 14 with the addition of 10% aqueous sodium hydroxide. A precipitate formed, was isolated by filtration, washed with water (3×100 mL), and dried overnight on the filter funnel to provide 7-bromo-1-(2-methylpropyl)-2-propyl-1H-imidazo[4,5-c]quinoline as an off-white solid.

来源