Reaktion #54851

Reaktionsgleichung

1,3,5-triphenyl-2-penten-1,5-dione

aniline

acetic acid

→

1,2,4,6-Tetraphenylpyridinium Acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeIn a suitable container (erlenmeyer flasks are suitable
2. 2
   Temperaturany other vessel which may be heated could
3. 3
   Temperaturheat on a steam bath
4. 4
   workup.ADDITIONAt the end of the heating period add 650 ml
5. 5
   workup.DISTILLATIONof distilled
6. 6
   workup.ADDITIONdeionized water and then add 6 N NaOH slowly with extremely rapid stirring
7. 7
   workup.ADDITIONthe addition when the pH
8. 8
   Sonstigecollect the supernate
9. 9
   Filtrationby filtration
10. 10
    workup.WAITto stand for a day
11. 11
    Filtrationfilter with 2 g of activated carbon by gravity through a tight filter paper
12. 12
    Sonstigeto produce a decolorized filtrate
13. 13
    EinengenAfter determination of the 1,2,4,6-tetraphenylpyridinium acetate concentration (vide infra)
14. 14
    workup.ADDITIONdilute the solution to the desired
15. 15
    Einengenconcentration
16. 16
    workup.DISTILLATIONwith distilled

Vorschrift

In a suitable container (erlenmeyer flasks are suitable but any other vessel which may be heated could serve as well) place 33.33 g of recrystallized 1,3,5-triphenyl-2-penten-1,5-dione and 9.31 g of purified aniline. To this mixture add 37.5 ml of glacial acetic acid and heat on a steam bath or other suitable heating source for two hours. At the end of the heating period add 650 ml of distilled, deionized water and then add 6 N NaOH slowly with extremely rapid stirring. Discontinue the addition when the pH, indicated by a glass electrode, reaches 7.0. Allow any precipitate to settle, collect the supernate by filtration and retain this filtrate. Allow the filtrate to stand for a day, and then filter with 2 g of activated carbon by gravity through a tight filter paper to produce a decolorized filtrate. After determination of the 1,2,4,6-tetraphenylpyridinium acetate concentration (vide infra) dilute the solution to the desired concentration with distilled, deionized water. The 1,2,4,6-tetraphenylpyridinium cation is characterized through its perchlorate and perrhenate salts by elemental analysis.

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