反应 #9571

ord-85819ad6c6834adb8e5accf545355994

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated
  2. 2
    温度at reflux overnight
  3. 3
    浓缩The reaction mixture was concentrated under reduced pressure
  4. 4
    其他the residue was purified by HPFC (
  5. 5
    洗涤eluting with chloroform

实验过程

A mixture of 5-bromo-N4-(2-methylpropyl)quinoline-3,4-diamine (1.0 g, 3.4 mmol), triethyl orthoformate (0.9 mL, 5 mmol), and pyridine hydrochloride (117 mg, 1.0 mmol) in acetonitrile (17 mL) was heated at reflux overnight. The reaction mixture was concentrated under reduced pressure, and the residue was purified by HPFC (eluting with chloroform:CMA in a gradient from 100:0 to 70:30) to provide 9-bromo-1-(2-methylpropyl)-1H-imidazo[4,5-c]quinoline as a dark oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07091214B2uspto-grants-2006_08