Methane → HCID 178427298, Verbindung

HRID 1704196

Reaktionsgleichung

Reaktionsgleichung von HRID 1704196
[C:1]1([CH3:13])[CH:6]=[CH:5][C:4]([S:7]([CH2:10][C:11]#[N:12])(=[O:9])=[O:8])=[CH:3][CH:2]=1.[N-:14]=[N+:15]=[N-:16].[Na+].[Cl-].[NH4+].C.Cl>CN(C)C=O>[C:1]1([CH3:13])[CH:2]=[CH:3][C:4]([S:7]([CH2:10][C:11]2[NH:16][N:15]=[N:14][N:12]=2)(=[O:8])=[O:9])=[CH:5][CH:6]=1

Komponenten

7

Edukt 5

HCID 297MethaneHCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 79776Tosylacetonitrile

Produkt 1

HCID 178427298HCID 178427298, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

97.5 parts of p-tolylsulphonyl-acetonitrile are stirred together with 39 parts of sodium azide, 32 parts of ammonium chloride and 200 parts of dimethylformamide for 10 hours at 120°-130° C. The dimethylformamide is distilled off in vacuo, and the residue is dissolved in 1000 parts of water with the addition of sodium hydroxide to give pH 9. The solution is treated with animal charcoal, and precipitation is effected at pH 2-3 by the addition of hydrochloric acid. Recrystallisation of the precipitate from isopropanol yields 85 parts of 5-(p-tolylsulphonylmethyl)-tetrazole in the form of white crystals which melt at 206°-208°.

Aufarbeitung

  1. distillationThe dimethylformamide is distilled off in vacuo
  2. dissolutionthe residue is dissolved in 1000 parts of water with the addition of sodium hydroxide
  3. customto give pH 9
  4. customRecrystallisation of the precipitate from isopropanol

Quellen und Nachweise

ORD-Eintrag
ord-ab7a75f7cb834f6bb853c2f1e5493b78
Quelldatensatz
uspto-grants-1978_11
Patentnummer
US04126590

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