Sodium Azide → HCID 178474793, Verbindung

HRID 1154118Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1154118
[C:1]([NH:4][CH2:5][CH2:6][CH2:7][NH:8][C:9](=[S:12])SC)(=[O:3])[CH3:2].[N-:13]=[N+:14]=[N-:15].[Na+]>O1CCOCC1.O>[C:1]([NH:4][CH2:5][CH2:6][CH2:7][N:8]1[C:9]([SH:12])=[N:15][N:14]=[N:13]1)(=[O:3])[CH3:2]

Komponenten

5

Edukt 2

HCID 33557Sodium AzideHCID 23324174Methyl (3-acetamidopropyl)carbamodithioate

Produkt 1

HCID 178474793HCID 178474793, VerbindungAusbeute 48,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A mixture of a solution of methyl N-(3-acetamidopropyl)dithiocarbamate (193 g) in dioxane (610 ml) and a solution of sodium azide (79.42 g) in water (500 ml) was refluxed under stirring for 4 hours. Dioxane was distilled off and the remaining aqueous layer was washed with diethyl ether (150 ml×2), adjusted to pH 1 with 17.5% hydrochloric acid, and cooled in an ice bath. Precipitates were collected by filtration and washed with ice-water to give white power of 1-(3-acetamidopropyl)-1H-tetrazol-5-thiol (91.75 g), mp. 152° to 154° C.

Aufarbeitung

  1. distillationDioxane was distilled off
  2. washthe remaining aqueous layer was washed with diethyl ether (150 ml×2)
  3. temperaturecooled in an ice bath
  4. customPrecipitates
  5. filtrationwere collected by filtration
  6. washwashed with ice-water

Quellen und Nachweise

ORD-Eintrag
ord-d6603d2565b04b7e8cb71b26df476537
Quelldatensatz
uspto-grants-1984_12
Patentnummer
US04487767

Notizen zur Reaktion

Wird geladen…