Reaktion #55473

Reaktionsgleichung

hydrogen chloride

2,6-dichloroaniline

HCl

m-cresol

sodium hydroxide

methyl cyanamide

→

1-(2,6-dichlorophenyl)-3-methylguanidine hydrochloride

Lösungsmittel

ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated on a steam bath
2. 2
   Temperaturthen heated for 2 hours on a steam bath
3. 3
   TemperaturThe reaction mixture is then cooled
4. 4
   Temperaturcooled
5. 5
   Extraktionextracted with 2 liters of ether
6. 6
   WaschenThe ether layer is washed with 2×1 liter of water
7. 7
   Trocknendried over sodium sulfate
8. 8
   Sonstigeevaporated
9. 9
   SonstigeThe residue is triturated with hexane
10. 10
    Filtrationthe precipitate is filtered off
11. 11
    Waschenwashed with ether
12. 12
    Sonstigedried

Vorschrift

To 51 g (0.315 mole) of 2,6-dichloroaniline is added 0.4 moles of ethereal HCl and 200 ml of m-cresol. The mixture is then stirred and heated on a steam bath to drive off the ether and excess hydrogen chloride. To the resultant mixture is then added 17.7 g (0.315 mole) of methyl cyanamide then heated for 2 hours on a steam bath. The reaction mixture is then cooled, added to 150 ml of conc. sodium hydroxide solution, cooled and extracted with 2 liters of ether. The ether layer is washed with 2×1 liter of water, dried over sodium sulfate, charcoaled and evaporated. The residue is triturated with hexane and the precipitate is filtered off and washed with ether and dried to obtain 1-(2,6-dichlorophenyl)-3-methylguanidine hydrochloride.

Quelle