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Thiosemicarbazide Hydrochloride → HCID 178491699, Verbindung

HRID 1089983
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1089983
C(O[C:4]1[CH2:8][CH:7]([S:9][CH2:10][C:11]2[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=2)[CH2:6][N:5]=1)C.Cl.[NH2:20][NH:21][C:22]([NH2:24])=[S:23]>C(O)C>[CH3:18][O:17][C:14]1[CH:15]=[CH:16][C:11]([CH2:10][S:9][CH:7]2[CH2:6][NH:5][C:4](=[N:20][NH:21][C:22]([NH2:24])=[S:23])[CH2:8]2)=[CH:12][CH:13]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 3037943Thiosemicarbazide HydrochlorideHCID 104680652-Ethoxy-4-p-methoxybenzylthio-1-pyroline

Produkt 1

HCID 178491699HCID 178491699, VerbindungAusbeute 21,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 2-ethoxy-4-p-methoxybenzylthio-1-pyrroline (900 mg) and thiosemicarbazide hydrochloride (433 mg) in ethanol (30 ml) was refluxed under heating for 1.5 hours. The reaction solution was evaporated to dryness under reduced pressure, then the residue was distributed between ethyl acetate and 5% aqueous solution of sodium hydroxide and the organic phase was dried over Na2SO4 before the solvent was distilled off under reduced pressure. The resultant residue was passed through a column packed with 25 g of silica gel and eluted with ethyl acetate and thus 230 mg of the objective compound was obtained as colorless foam.

Aufarbeitung

  1. temperatureunder heating for 1.5 hours
  2. customThe reaction solution was evaporated to dryness under reduced pressure
  3. dry with materialthe organic phase was dried over Na2SO4 before the solvent
  4. distillationwas distilled off under reduced pressure
  5. washeluted with ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-2989a10ea17346a48096364ba1fbac48
Quelldatensatz
uspto-grants-1992_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05079357

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