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Pyridine → 5-Phenyl-1H-pyrrole-3-carbonitrile

HRID 1651694
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1651694
[C:1]1([C:7]2[CH2:11][CH:10]([C:12]#[N:13])[CH2:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.N1C=CC=CC=1>COCCOC>[C:1]1([C:7]2[NH:8][CH:9]=[C:10]([C:12]#[N:13])[CH:11]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 1049PyridineHCID 12294966HCID 12294966, Verbindung

Produkt 1

HCID 100807675-Phenyl-1H-pyrrole-3-carbonitrileAusbeute 59,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 80711,2-DimethoxyethaneLösungsmittel

Versuchsvorschrift

Under a nitrogen purge 2,3-dichloro-5,6-dicyano-1,4-bonzoquinone (0.23 g; 0.001 mol) and 2-phenyl-1-pyrroline-4-carbonitrile (0.17 g; 0.001 mol) is dissolved in 1,2-dimethoxyethane (13 mL) to form a clear orange solution. Pyridine (0.08 mL; 0,001 mol) is added in a single portion, causing a slight exotherm (to ca. 28° C.) and an immediate formation of a green/grey precipitate. The suspension is stirred at room temperature for 18 hours during which time much of the solvent evaporates. The brownish semi-solid residue is partitioned between ether and a half-saturated solution of sodium carbonate. The red-brown aqueous layer is extracted twice with ether and the combined ether layer is washed with fresh water, then saturated sodium chloride. After drying with MgSO4, solvent is removed under reduced pressure to obtain a white semi-solid. This material was recrystallized from ethylene dichloride (DARCO treatment) to yield lavender crystals (0.1 g).

Aufarbeitung

  1. customto form a clear orange solution
  2. customa slight exotherm (to ca. 28° C.)
  3. customevaporates
  4. customThe brownish semi-solid residue is partitioned between ether
  5. extractionThe red-brown aqueous layer is extracted twice with ether
  6. washthe combined ether layer is washed with fresh water
  7. dry with materialAfter drying with MgSO4, solvent
  8. customis removed under reduced pressure
  9. customto obtain a white semi-solid
  10. customThis material was recrystallized from ethylene dichloride (DARCO treatment)

Quellen und Nachweise

ORD-Eintrag
ord-adac08e57fee459398597d51ea90609b
Quelldatensatz
uspto-grants-1990_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04929634

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