Sodium Azide → HCID 178468987, Verbindung

HRID 2119121

Reaktionsgleichung

Reaktionsgleichung von HRID 2119121
[C:1]([C:6]1[CH:11]=[CH:10][C:9]([N:12]=[C:13]=[S:14])=[CH:8][CH:7]=1)([O:3][CH2:4][CH3:5])=[O:2].[N-:15]=[N+:16]=[N-:17].[Na+]>O>[C:1]([C:6]1[CH:11]=[CH:10][C:9]([N:12]2[C:13]([SH:14])=[N:17][N:16]=[N:15]2)=[CH:8][CH:7]=1)([O:3][CH2:4][CH3:5])=[O:2]

Komponenten

4

Edukt 2

HCID 33557Sodium AzideHCID 71003Ethyl 4-isothiocyanatobenzoate

Produkt 1

HCID 178468987HCID 178468987, VerbindungAusbeute 55 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

20 g of 4-carboethoxyphenyl isothiocyanate and 6.5 g of sodium azide are added to water and heated at 80° C. After 2 hours of reaction, the reaction mixture is filtered, cooled and acidified with hydrochloric acid to give crystals of 1-(4-carboethoxyphenyl)-5-mercaptotetrazole. To the crystals are added 5 equivalents of sodium hydroxide (1N NaOH in water) and the mixture is heated at 80° C. for 5 hours. After cooling, the reaction mixture is acidified with hydrochloric acid to cause crude crystals of Compound III-4 to separate out. The crystals are recrystallized from methanol. Yield: 55%, m.p. about 195° C. (decomposed).

Aufarbeitung

  1. customAfter 2 hours of reaction
  2. filtrationthe reaction mixture is filtered
  3. temperaturecooled

Quellen und Nachweise

ORD-Eintrag
ord-1c4da6bcbb5c45cc9fd00fda92d2504c
Quelldatensatz
uspto-grants-1987_07
Patentnummer
US04683189

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