Ethanol → HCID 178512100, Verbindung

HRID 2419778

Reaktionsgleichung

Reaktionsgleichung von HRID 2419778
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.[CH2:17]([NH2:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C(O)C>O>[CH2:17]([NH:24][C:8]([NH:7][N:6]=[CH:5][C:4]1[C:12]([Cl:16])=[CH:13][CH:14]=[CH:15][C:3]=1[Cl:2])=[NH:11])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

Komponenten

5

Edukt 3

HCID 702EthanolHCID 7504BenzylamineHCID 178504060Methyl 3-(2,6-dichlorobenzylidene)thiocarbazimidate hydroiodide

Produkt 1

HCID 178512100HCID 178512100, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 93.6 g of methyl 3-(2,6-dichlorobenzylidene)thiocarbazimidate hydroiodide (U.S. Pat. No. 3,657,337) and 51.2 of benzylamine in 400 ml. of absolute ethanol is heated at reflux for 6 hours and then diluted while hot with 400 ml. of water, causing the separation of an oil. On standing, the oil crystallizes and the nearly colorless crystals are recovered by filtration. Recrystallization from aqueous ethanol gives the desired product as pale yellow crystals, m.p. 134°-137° C.

Aufarbeitung

  1. temperatureat reflux for 6 hours
  2. additiondiluted while hot with 400 ml
  3. customthe separation of an oil
  4. customthe oil crystallizes
  5. filtrationthe nearly colorless crystals are recovered by filtration
  6. customRecrystallization from aqueous ethanol

Quellen und Nachweise

ORD-Eintrag
ord-1d5415641c3a4837909b31b0e8f6a582
Quelldatensatz
uspto-grants-1978_08
Patentnummer
US04107326

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