反应 #554567

ord-efba66156385427dbe80e4808b229765

反应方程式

O=P(Cl)(Cl)Cl
Phosphorus oxychloride
CN(C)c1ccccc1
dimethylaniline
c1ccc2c(c1)cnc1ccccc12
phenanthridine
Clc1ccc2cnc3ccccc3c2c1
9-chlorophenanthridine
收率 96.0%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度by refluxing for 3 hours
  2. 2
    萃取the obtained solid was extracted with chloroform
  3. 3
    干燥by drying with sodium sulfate
  4. 4
    过滤After filtration
  5. 5
    其他the filtrate was evaporated to dryness under reduced pressure
  6. 6
    其他The obtained solid was purified by column chromatography (eluent: chloroform) (amount: 2.1 g, yield: 96%)

实验过程

Phosphorus oxychloride (15 ml) and dimethylaniline (0.63 ml) were added to phenanthridine (2.0 g), followed by refluxing for 3 hours. The solution was poured into H2O to generate a solid, and the obtained solid was extracted with chloroform, followed by drying with sodium sulfate. After filtration, the filtrate was evaporated to dryness under reduced pressure. The obtained solid was purified by column chromatography (eluent: chloroform) (amount: 2.1 g, yield: 96%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08623239B2uspto-grants-2014_01