Diphenylcyclopropenone → HCID 21462217, Verbindung

HRID 1940457Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1940457
[C:1]1([C:7]2[C:9](=[O:10])[C:8]=2[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:17]([C:19]1[CH:20]=[N:21][CH:22]=[CH:23][C:24]=1[C:25]#[N:26])#[N:18]>ClC1C=CC=CC=1>[OH:10][C:9]1[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[C:8]([C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)[N:21]2[C:22]=1[CH:23]=[C:24]([C:25]#[N:26])[C:19]([C:17]#[N:18])=[CH:20]2

Komponenten

4

Edukt 2

HCID 65057DiphenylcyclopropenoneHCID 74211Pyridine-3,4-dicarbonitrile

Produkt 1

HCID 21462217HCID 21462217, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7964ChlorobenzeneLösungsmittel

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

Diphenylcyclopropenone (0.319 g, 1.55 mmol) and 3,4-dicyanopyridine (0.200 g, 1.55 mmol) were mixed in a dry, argon filled reaction flask. Chlorobenzene (2.5 mL) (oxygen free) was added, and the reaction was heated to 130° C. After 2 h the heating was stopped and the reaction was allowed to reach room temperature. Petroleum ether 40°-60° C. (2.5 mL) was added in order to obtain a complete precipitate of the product. The solvent was filtered off and the precipitate was washed with petroleum ether. The crude product was stirred with chloroform (30 mL) for 1 h. The dark chloroform solution was filtered off leaving the title product as a yellow precipitate.

Aufarbeitung

  1. additionfilled
  2. customreaction flask
  3. customto reach room temperature
  4. customto obtain a complete precipitate of the product
  5. filtrationThe solvent was filtered off
  6. washthe precipitate was washed with petroleum ether
  7. filtrationThe dark chloroform solution was filtered off

Quellen und Nachweise

ORD-Eintrag
ord-9781798653424b4ba33cd5b33f8b2136
Quelldatensatz
uspto-grants-1997_12
Patentnummer
US05700448

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