Reaktion #172508

Reaktionsgleichung

4-(dibutylamino)-2-methoxybenzaldehyde

1,3-bis(dicyanomethylidene)indan

water

→

black crystal

Ausbeute 86.5%

2-[2-(4-dibutylamino-2-methoxybenzylidene)-3-dicyanomethyleneindan-1-ylidene]malonnitrile

Ausbeute 86.5%

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe precipitate was separated by filtration
2. 2
   Waschenwashed with water
3. 3
   Sonstigedried
4. 4
   SonstigeThe crystal was purified by silica gel column chromatography
5. 5
   Waschenwashed with methanol

Vorschrift

In 10 ml of anhydrous acetic acid were dissolved 0.8 g (3.04 mmol) of 4-(dibutylamino)-2-methoxybenzaldehyde and 0.73 g (3.01 mmol) of 1,3-bis(dicyanomethylidene)indan. The mixture was stirred with heating at 80° C. for 2 hours. The reaction mixture was poured into 200 ml of water and the precipitate was separated by filtration, washed with water, and dried. The crystal was purified by silica gel column chromatography and washed with methanol to give 1.27 g of a black crystal having a mp of 195-198° C. (yield: 86.4%).

Quelle