تفاعل #554567

ord-efba66156385427dbe80e4808b229765

معادلة التفاعل

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

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةby refluxing for 3 hours
  2. 2
    استخلاصthe obtained solid was extracted with chloroform
  3. 3
    تجفيفby drying with sodium sulfate
  4. 4
    ترشيحAfter filtration
  5. 5
    أخرىthe filtrate was evaporated to dryness under reduced pressure
  6. 6
    أخرىThe obtained solid was purified by column chromatography (eluent: chloroform) (amount: 2.1 g, yield: 96%)

الإجراء التجريبي

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%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08623239B2uspto-grants-2014_01