Reaktion #354506

Reaktionsgleichung

1,3-diaminoguanidine hydrochloride

sodium hydroxide

4-chlorobenzaldehyde

ethanol

ethanol

→

1-Amino-3-(4-chlorobenzylideneamino)guanidine Hydrochloride

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe preparation of the subject compound
2. 2
   Einengenthe filtrate concentrated to 500 ml
3. 3
   Temperaturvolume and cooled at 0°C
4. 4
   Sonstigeof precipitate is obtained
5. 5
   Temperaturthe slurry heated
6. 6
   Filtrationfiltered
7. 7
   TemperaturCooling
8. 8
   Sonstigefiltrate gives 18 g

Vorschrift

The preparation of the subject compound may also be accomplished as follows: 25 g. of 1,3-diaminoguanidine hydrochloride is dissolved in 1800 ml. of boiling ethanol. To this boiling solution, 28 g. of 4-chlorobenzaldehyde in 300 ml. of ethanol is added over a period of 8 hours. The reaction mixture is then cooled at 0°C. overnight, clarified, and the filtrate concentrated to 500 ml. volume and cooled at 0°C. 29 g. of precipitate is obtained. This is slurried in 300 ml. of water, the pH adjusted to 8-8.5 with sodium hydroxide solution, the slurry heated to boiling and filtered. Cooling and filtrate gives 18 g. of essentially pure product melting at 243°-244°C., as in the previous preparation.

Quelle