반응 #554567

ord-efba66156385427dbe80e4808b229765

반응 방정식

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

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도by refluxing for 3 hours
  2. 2
    추출the obtained solid was extracted with chloroform
  3. 3
    건조by drying with sodium sulfate
  4. 4
    여과After filtration
  5. 5
    기타the filtrate was evaporated to dryness under reduced pressure
  6. 6
    기타The obtained solid was purified by column chromatography (eluent: chloroform) (amount: 2.1 g, yield: 96%)

실험 절차

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08623239B2uspto-grants-2014_01