Ethyl Bromide → 4-Vinylphenethylammonium bromide

HRID 1106131

Reaktionsgleichung

Reaktionsgleichung von HRID 1106131
C([N:3]([CH2:6][CH2:7][C:8]1[CH:15]=[CH:14][C:11]([CH:12]=[CH2:13])=[CH:10][CH:9]=1)CC)C.C([Br:18])C>CO>[Br-:18].[CH:12]([C:11]1[CH:14]=[CH:15][C:8]([CH2:7][CH2:6][NH3+:3])=[CH:9][CH:10]=1)=[CH2:13]

Komponenten

4

Edukt 2

HCID 6332Ethyl BromideHCID 3015378N,N-Diethyl-p-vinylphenethylamine

Produkt 1

HCID 205545994-Vinylphenethylammonium bromide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

All the procedures were conducted in a dry nitrogen atmosphere since the product was extremely hygroscopic. In a 100 ml two necked flask equipped with a three way cock 8.6 g of the p-diethylaminoethylstyrene as obtained in Synthesis 1 were dissolved in 35 ml of absolute methanol and then 12.7 ml of ethyl bromide were injected via a syringe. The quaternization was completed after 48 hours at 40° C. without any side reactions. After the reaction mixture was concentrated under reduced pressure, 100 ml of ethyl acetate were injected via a syringe to immediately precipitate white crystals. The crystals thus formed were separated from the solution by filtration under a dry nitrogen atmosphere, washed with ethyl acetate, dried in vacuum and recrystallized from methanol-ethyl acetate solution. The results of elemental analysis of the crystals are as follows;

Aufarbeitung

  1. customas obtained in Synthesis 1
  2. concentrationAfter the reaction mixture was concentrated under reduced pressure, 100 ml of ethyl acetate
  3. customwere injected via a syringe to immediately precipitate white crystals
  4. customThe crystals thus formed
  5. customwere separated from the solution by filtration under a dry nitrogen atmosphere
  6. washwashed with ethyl acetate
  7. customdried in vacuum
  8. customrecrystallized from methanol-ethyl acetate solution
  9. customThe results of elemental analysis of the crystals

Quellen und Nachweise

ORD-Eintrag
ord-b152447a8ebb427e9a412968d72c6538
Quelldatensatz
uspto-grants-1982_01
Patentnummer
US04311799

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