Reaktion #551145

Reaktionsgleichung

Benzil

cyanoacetohydrazide

→

4-Cyano-5,6-diphenyl-3-(2H)-pyridazinone

Ausbeute 95.0%

Lösungsmittel

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe solution was cooled
2. 2
   Filtrationthe precipitant solid was filtered
3. 3
   Waschenwashed with ethyl alcohol
4. 4
   workup.DISTILLATIONdistilled
5. 5
   Waschenthe residual solid was washed with ethyl alcohol
6. 6
   Filtrationfiltered
7. 7
   SonstigeThere was isolated 74.5 grams

Vorschrift

Benzil 63.1 grams (0.3 mole) along with 30 grams (0.3 mole) of cyanoacetohydrazide in 200 mls of dimethylformamide was heated at 110° C. for five hours. The solution was cooled and the precipitant solid was filtered and washed with ethyl alcohol. The filtrate was vacuum distilled and the residual solid was washed with ethyl alcohol and filtered. There was isolated 74.5 grams, a 95% yield, of a solid which melted at 280°-281° C. Calculated for C17H11N3O, C, 74.7; H, 4.1; N, 15.4. Found: C, 74.4; H, 4.16; N, 15.2. The infrared spectra showed the nitrile at 4.5μ; the ##STR57## band for an amide at 6.0μ.

Quelle