Ethanol → 1-(2,6-Dichlorobenzylideneamino)-3-(2-pyridylmethyl)guanidine

HRID 262763

Reaktionsgleichung

Reaktionsgleichung von HRID 262763
I.[Cl:2][C:3]1[CH:15]=[CH:14][CH:13]=[C:12]([Cl:16])[C:4]=1[CH:5]=[N:6][NH:7][C:8](=[NH:11])SC.[NH2:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=1.C(O)C>O>[Cl:2][C:3]1[CH:15]=[CH:14][CH:13]=[C:12]([Cl:16])[C:4]=1[CH:5]=[N:6][NH:7][C:8]([NH:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=1)=[NH:11]

Komponenten

5

Edukt 3

HCID 702EthanolHCID 195092-PyridinemethanamineHCID 178504060Methyl 3-(2,6-dichlorobenzylidene)thiocarbazimidate hydroiodide

Produkt 1

HCID 1785121061-(2,6-Dichlorobenzylideneamino)-3-(2-pyridylmethyl)guanidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 5.85 g. of methyl 3-(2,6-dichlorobenzylidene)thiocarbazimidate hydriodide (U.S. Pat. No. 3,657,337) and 3.24 g. of 2-(aminomethyl)pyridine in 25 ml. of absolute ethanol is heated under reflux for 20 hours and diluted while hot with 75 ml. of water, causing the separation of an oil. On standing, the oil crystallizes and filtration gives 5.00 g. of pale yellow crystals, m.p. 125°-140° C. Recrystallization from aqueous ethanol gives the desired compound as pale yellow crystals, m.p. 159.5°-161° C.

Aufarbeitung

  1. temperatureunder reflux for 20 hours
  2. additiondiluted while hot with 75 ml
  3. customthe separation of an oil
  4. customthe oil crystallizes
  5. filtrationfiltration
  6. customgives 5.00 g
  7. customRecrystallization from aqueous ethanol

Quellen und Nachweise

ORD-Eintrag
ord-e355e821ec8245679c76df6f123e72ba
Quelldatensatz
uspto-grants-1979_05
Patentnummer
US04154947

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