Reaktion #52204

Reaktionsgleichung

sulphanilamide

benzoyl cyanamide

→

crude title product

4-Sulphamoylphenylguanidine

Lösungsmittel

ethanol

hydrochloric acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated on a steam bath until the solvent
2. 2
   Sonstigehad evaporated
3. 3
   workup.ADDITIONWater was added
4. 4
   Temperaturthe mixture heated
5. 5
   Temperaturat reflux for 5 minutes
6. 6
   workup.ADDITIONSodium hydroxide (14.4 g) was added
7. 7
   Temperaturthe mixture heated
8. 8
   Temperaturat reflux
9. 9
   Temperaturto cool
10. 10
    Sonstigethe precipitated solid removed by filtration
11. 11
    Sonstigethe solvent removed by evaporation
12. 12
    SonstigeThe residue was recrystallized from water

Vorschrift

A mixture of sulphanilamide (20 g, 0.166 mol), benzoyl cyanamide (34 g, 0.33 mmol) in ethanol (60 ml) and concentrated hydrochloric acid (11 ml) was heated on a steam bath until the solvent had evaporated. Water was added and the mixture heated at reflux for 5 minutes. Sodium hydroxide (14.4 g) was added and the mixture heated at reflux. The mixture was allowed to cool and was adjusted to pH2 with hydrochloric acid and the precipitated solid removed by filtration. The filtrate was neutralised and the solvent removed by evaporation. The residue was recrystallized from water to give crude title product. m/z: 215 [MH]+.

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