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Sodium Hydroxide → HCID 178526006, Verbindung

HRID 904868
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 904868
[C:1]([CH2:6][N:7]1[C:11]([SH:12])=[N:10][N:9]=[N:8]1)([C:3]([OH:5])=[O:4])=[O:2].[OH-].[Na+]>C(O)C.[Zn]>[C:3]([CH:1]([OH:2])[CH2:6][N:7]1[C:11]([SH:12])=[N:10][N:9]=[N:8]1)([OH:5])=[O:4]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 14798Sodium HydroxideHCID 178526005HCID 178526005, Verbindung

Produkt 1

HCID 178526006HCID 178526006, VerbindungAusbeute 42,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23994ZincKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

1-Oxalomethyl-1H-tetrazole-5-thiol (0.94 g) was dissolved in aqueous 60% ethanol (15 ml) containing sodium hydroxide (1.4 g) and to this solution was added portionwise zinc powder (0.98 g). The mixture was stirred at room temperature for 3.5 hours. After removal of zinc powder by filtration, ethanol was removed under reduced pressure and the remained aqueous solution was adjusted to pH 2.0 with 10% hydrochloric acid. Extraction with ethyl acetate, drying over magnesium sulfate and evaporation gave an oil which was triturated with a mixture of diisopropyl ether and n-hexane (1:1). The crystals were filtered and washed with a mixture of diisopropyl ether and n-hexane (1:1) to give 1-(2-carboxy-2-hydroxyethyl)-1H-tetrazole-5-thiol (0.40 g), mp 143° to 146° C.,

Aufarbeitung

  1. customAfter removal of zinc powder
  2. filtrationby filtration, ethanol
  3. customwas removed under reduced pressure
  4. extractionExtraction with ethyl acetate
  5. dry with materialdrying over magnesium sulfate and evaporation
  6. customgave an oil which
  7. customwas triturated with a mixture of diisopropyl ether and n-hexane (1:1)
  8. filtrationThe crystals were filtered
  9. washwashed with a mixture of diisopropyl ether and n-hexane (1:1)

Quellen und Nachweise

ORD-Eintrag
ord-f2c48d0e1e7a47618fdc41b2e1a91011
Quelldatensatz
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04420477

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