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Hydrochloric Acid → HCID 178526005, Verbindung

HRID 904865
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 904865
[C:1]([CH2:8][N:9]1[C:13]([SH:14])=[N:12][N:11]=[N:10]1)([C:3]([O:5]CC)=[O:4])=[O:2].[OH-].[Na+].Cl>CO>[C:1]([CH2:8][N:9]1[C:13]([SH:14])=[N:12][N:11]=[N:10]1)([C:3]([OH:5])=[O:4])=[O:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 178473105HCID 178473105, Verbindung

Produkt 1

HCID 178526005HCID 178526005, VerbindungAusbeute 59,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of 1-ethoxalylmethyl-1H-tetrazole-5-thiol (18.6 g) in methanol (186 ml) was added 1 N aqueous solution of sodium hydroxide (172 ml) at room temperature and the mixture was stirred for 40 minutes. After adjusting to pH 7.5 with 10% hydrochloric acid, the solution was evaporated in vacuo to remove methanol and the remained aqueous solution was washed with ethyl acetate (100 ml). The aqueous solution was adjusted to pH 4.0 and washed again with ethyl acetate to remove impurities. The aqueous solution was adjusted to pH 2.5, and extracted with ethyl acetate, dried over magnesium sulfate and evaporated to give pale yellow powder of 1-oxalomethyl-1H-tetrazole-5-thiol (9.7 g), mp 140° to 150° C. (dec.).

Aufarbeitung

  1. customthe solution was evaporated in vacuo
  2. customto remove methanol
  3. washthe remained aqueous solution was washed with ethyl acetate (100 ml)
  4. washwashed again with ethyl acetate
  5. customto remove impurities
  6. extractionextracted with ethyl acetate
  7. dry with materialdried over magnesium sulfate
  8. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-7b9f650e7193436f84931167e2749483
Quelldatensatz
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04420477

Notizen zur Reaktion

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