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Water → HCID 178505113, Verbindung

HRID 866880
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 866880
[N+](C1C=C([N+]([O-])=O)C=CC=1[S:13][C:14]1[N:18]([CH2:19][CH2:20][NH:21][S:22]([CH3:25])(=[O:24])=[O:23])[N:17]=[N:16][N:15]=1)([O-])=O.C[O-].[Na+].O>CO>[CH3:25][S:22]([NH:21][CH2:20][CH2:19][N:18]1[C:14]([SH:13])=[N:15][N:16]=[N:17]1)(=[O:24])=[O:23]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 962WaterHCID 10942334Sodium MethoxideHCID 203186985-(2,4-Dinitrophenylthio)-1-(2-methanesulfonamidoethyl)tetrazole

Produkt 1

HCID 178505113HCID 178505113, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

5-(2,4-Dinitrophenylthio)-1-(2-methanesulfonamidoethyl)tetrazole (4.46 g, 11.5 mmol) was added to 60 ml of 5% sodium methoxide in methanol. After 1 hour, water was added and the solid material was removed by filtration. The filtrate was concentrated in vacuo and 3N hydrochloric acid was added to the residue to bring the pH to 1.4. The acidic solution was filtered and the filtrate was extracted twice with ethyl acetate. The extracts were combined and concentrated to give a residue which crystallized upon addition of ethyl acetate to give 1-(2-methanesulfonamidoethyl)tetrazole-5-thiol, mp 131°-132°.

Aufarbeitung

  1. customthe solid material was removed by filtration
  2. concentrationThe filtrate was concentrated in vacuo and 3N hydrochloric acid
  3. additionwas added to the residue
  4. filtrationThe acidic solution was filtered
  5. extractionthe filtrate was extracted twice with ethyl acetate
  6. concentrationconcentrated
  7. customto give a residue which
  8. customcrystallized upon addition of ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-ed6ee3a967bd4b89a6bff7bd3895eb53
Quelldatensatz
uspto-grants-1978_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04101656

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