Diphenylcyclopropenone → HCID 21462217, Verbindung

HRID 1648159Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1648159
[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

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 130C. After 2 h the heating was stopped and the reaction was allowed to reach room temperature. Petroleum ether 40-60C (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 lb. 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-2bd5c21322c742cfb57ecb786c08207f
Quelldatensatz
uspto-grants-1995_07
Patentnummer
US05435991

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