Reaktionsgleichung
[Cl:1][C:2]1[CH:8]=[CH:7][CH:6]=[C:5]([Cl:9])[C:3]=1[NH2:4].Cl.C1C(O)=CC=CC=1C.[CH3:19][NH:20][C:21]#[N:22].[OH-].[Na+]>CCOCC>[ClH:1].[Cl:1][C:2]1[CH:8]=[CH:7][CH:6]=[C:5]([Cl:9])[C:3]=1[NH:4][C:21]([NH:20][CH3:19])=[NH:22]Komponenten
Edukt 5
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
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 sitrred 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.
Aufarbeitung
- temperatureheated on a steam bath
- temperaturethen heated for 2 hours on a steam bath
- temperatureThe reaction mixture is then cooled
- temperaturecooled
- extractionextracted with 2 liters of ether
- washThe ether layer is washed with 2×1 liter of water
- dry with materialdried over sodium sulfate
- customevaporated
- customThe residue is triturated with hexane
- filtrationthe precipitate is filtered off
- washwashed with ether
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-c4328a3f764f40b6a388b4a2152e3b6e
- Quelldatensatz
- uspto-grants-1984_12
- Patentnummer
- US04488993
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