Hydrochloric Acid → HCID 178479391, Verbindung

HRID 1154284

Reaktionsgleichung

Reaktionsgleichung von HRID 1154284
[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.[N:19]#[C:20][NH2:21].[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:20]([NH2:21])=[NH:19]

Komponenten

7

Edukt 5

HCID 313Hydrochloric Acid2×HCID 342M-CresolHCID 9864CyanamideHCID 118462,6-DichloroanilineHCID 14798Sodium Hydroxide

Produkt 1

HCID 178479391HCID 178479391, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

To 51 g (0.315 mole) of 2,6-dichloroaniline is added 0.4 moles of ethereal HCl and 200 l 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 13.3 g (0.315 mole) of 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 2,6-dichlorophenylguanidine hydrochloride.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-a2195f0a7320456a820efafb73b9d344
Quelldatensatz
uspto-grants-1984_12
Patentnummer
US04488993

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