Реакция #554567

ord-efba66156385427dbe80e4808b229765

Уравнение реакции

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

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураby refluxing for 3 hours
  2. 2
    Экстракцияthe obtained solid was extracted with chloroform
  3. 3
    Сушкаby drying with sodium sulfate
  4. 4
    ФильтрацияAfter filtration
  5. 5
    Другоеthe filtrate was evaporated to dryness under reduced pressure
  6. 6
    ДругоеThe obtained solid was purified by column chromatography (eluent: chloroform) (amount: 2.1 g, yield: 96%)

Методика

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%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08623239B2uspto-grants-2014_01