1H-1,2,4-Triazole → HCID 20030420, Verbindung

HRID 231978Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 231978
CC(C)([O-])C.[K+].[NH:7]1[CH:11]=[N:10][CH:9]=[N:8]1.[CH2:12]([S:19][C:20]1[CH:27]=[CH:26][CH:25]=[CH:24][C:21]=1[CH2:22]Cl)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>CN(C=O)C>[C:13]1([CH2:12][S:19][C:20]2[CH:27]=[CH:26][CH:25]=[CH:24][C:21]=2[CH2:22][N:7]2[CH:11]=[N:10][CH:9]=[N:8]2)[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

Komponenten

5

Edukt 3

HCID 92571H-1,2,4-TriazoleHCID 125079034521-46-4HCID 23665647Potassium tert-butoxide

Produkt 1

HCID 20030420HCID 20030420, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel2×

Versuchsvorschrift

To a suspension of 9.9 g of potassium t-butoxide in 100 ml of DMF under a N2 atmosphere was added portion wise 6 g of 1,2,4-triazole. After stirring at ambient temperature for one hour, a solution of 20 g of 2-benzylmercaptobenzyl chloride in 15 ml of DMF was added dropwise and the suspension was heated at 70° C. for 4 hours, then stirred at 25° C. 16 hours. After pouring the suspension into excess ice-water the residue was extracted with methylene chloride, dried (MgSO4), and the solvent was evaporated in vacuo to an oil residue which solidified to 14.5 g of the subject compound when triturated with 1-chlorobutane; m.p. 65°-68° C.

Aufarbeitung

  1. temperaturethe suspension was heated at 70° C. for 4 hours
  2. stirringstirred at 25° C
  3. custom16 hours
  4. extractionwas extracted with methylene chloride
  5. dry with materialdried (MgSO4)
  6. customthe solvent was evaporated in vacuo to an oil residue which
  7. customtriturated with 1-chlorobutane

Quellen und Nachweise

ORD-Eintrag
ord-f568b0db92384d55b41b21379eb997ab
Quelldatensatz
uspto-grants-1989_07
Patentnummer
US04851030

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