Water → HCID 178521269, Verbindung

HRID 1395786Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1395786
[OH:1][CH2:2][CH2:3][NH:4][C:5](=[S:8])SC.[N-:9]=[N+:10]=[N-:11].[Na+].O>O1CCOCC1>[OH:1][CH2:2][CH2:3][N:4]1[C:5]([SH:8])=[N:11][N:10]=[N:9]1

Komponenten

5

Edukt 3

HCID 962WaterHCID 33557Sodium AzideHCID 13277332Methyl (2-hydroxyethyl)carbamodithioate

Produkt 1

HCID 178521269HCID 178521269, VerbindungAusbeute 4,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A mixture of methyl N-(2-hydroxyethyl)dithiocarbamate (3.7 g.), sodium azide (2.4 g.), water (20 ml.) and dioxane (20 ml.) was heated under reflux for four hours. After the dioxane was removed from the mixture under reduced pressure, the aqueous solution was washed with ether. The solution was adjusted to pH 1 with 10% hydrochloric acid and extracted with ethyl acetate. The extract was concentrated under reduced pressure to give oily product (0.47 g.). The oily product was purified by column chromatography on silica gel to give 1-(2-hydroxyethyl)-1H-tetrazole-5-thiol (0.17 g.). m.p. 135° to 137° C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for four hours
  3. customAfter the dioxane was removed from the mixture under reduced pressure
  4. washthe aqueous solution was washed with ether
  5. extractionextracted with ethyl acetate
  6. concentrationThe extract was concentrated under reduced pressure
  7. customto give oily product (0.47 g.)
  8. customThe oily product was purified by column chromatography on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-048e4b2c16414efa996fe87eb4bac4e8
Quelldatensatz
uspto-grants-1980_05
Patentnummer
US04205166

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