Hydrochloric Acid → HCID 178485094, Verbindung

HRID 1764193

Reaktionsgleichung

Reaktionsgleichung von HRID 1764193
[CH3:1][C:2]1[CH:8]=[CH:7][CH:6]=[C:5]([CH3:9])[C:3]=1[NH2:4].Cl.C1C(O)=CC=CC=1C.[CH3:19][NH:20][C:21]#[N:22].[OH-].[Na+]>CCOCC>[CH3:1][C:2]1[CH:8]=[CH:7][CH:6]=[C:5]([CH3:9])[C:3]=1[NH:4][C:21]([NH:20][CH3:19])=[NH:22]

Komponenten

7

Edukt 5

HCID 313Hydrochloric Acid2×HCID 342M-CresolHCID 68962,6-DimethylanilineHCID 14798Sodium HydroxideHCID 119415Methylcyanamide

Produkt 1

HCID 178485094HCID 178485094, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

To 40.5 g. (0.315 mole) of 2,6-dimethylaniline 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-dimethylphenyl)-3-methylguanidine.

Aufarbeitung

  1. temperatureheated on a steam bath
  2. temperatureThe reaction mixture is then cooled
  3. additionadded to 150 ml
  4. extractionextracted with 2 liters of ether
  5. washThe ether layer is washed with 2 × 1 liter of water
  6. dry with materialdried over sodium sulfate
  7. customevaporated
  8. customThe residue is triturated with hexane
  9. filtrationthe precipitate is filtered off
  10. washwashed with ether
  11. customdried

Quellen und Nachweise

ORD-Eintrag
ord-530d85acb7f34857bc7c576be77247ae
Quelldatensatz
uspto-grants-1978_09
Patentnummer
US04115564

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