Ethanol → o-Tolyl thiosemicarbazide

HRID 2071228

Reaktionsgleichung

Reaktionsgleichung von HRID 2071228
Cl.[C:2]1([CH3:10])[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][NH2:9].[S-:11][C:12]#[N:13].[NH4+].C(O)C>O>[C:2]1([CH3:10])[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][NH:9][C:12]([NH2:13])=[S:11]

Komponenten

5

Edukt 3

HCID 702EthanolHCID 15666Ammonium thiocyanateHCID 71554o-Tolylhydrazinium(1+) chloride

Produkt 1

HCID 1490896o-Tolyl thiosemicarbazide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 15.9 g. (0.1 moles) of o-tolylhydrazine hydrochloride, 15.2 g. (0.2 moles) of ammonium thiocyanate, 300 ml. of ethanol and 30 ml. of water are heated at reflux temperature for 24 hours, the solvent is removed by distillation at atmospheric pressure, and sufficient water added to cause precipitation. The aqueous suspension is filtered and the solid residue recrystallized from aqueous ethanol affording 15 g. (85%) of 1-(o-tolyl)-3-thiosemicarbazide, m.p. 158°-160° C.

Aufarbeitung

  1. additionA mixture of 15.9 g
  2. temperatureat reflux temperature for 24 hours
  3. customthe solvent is removed by distillation at atmospheric pressure, and sufficient water
  4. additionadded
  5. customprecipitation
  6. filtrationThe aqueous suspension is filtered
  7. customthe solid residue recrystallized from aqueous ethanol affording 15 g

Quellen und Nachweise

ORD-Eintrag
ord-99d48bbfe556493a9025b89db86312d9
Quelldatensatz
uspto-grants-1977_09
Patentnummer
US04046753

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