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Triethylamine → 1-Dipropylcarbamoyl-3-propylsulphonyl-1,2,4-triazole

HRID 1606046
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1606046
[CH2:1]([N:4]([CH2:8][CH2:9][CH3:10])[C:5](Cl)=[O:6])[CH2:2][CH3:3].[CH2:11]([S:14]([C:17]1[N:21]=[CH:20][NH:19][N:18]=1)(=[O:16])=[O:15])[CH2:12][CH3:13].C(N(CC)CC)C>O1CCCC1>[CH2:1]([N:4]([CH2:8][CH2:9][CH3:10])[C:5]([N:19]1[CH:20]=[N:21][C:17]([S:14]([CH2:11][CH2:12][CH3:13])(=[O:16])=[O:15])=[N:18]1)=[O:6])[CH2:2][CH3:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 3015348Dipropylcarbamoyl chlorideHCID 1784610153-Propylsulphonyl-1,2,4-triazole

Produkt 1

HCID 203549701-Dipropylcarbamoyl-3-propylsulphonyl-1,2,4-triazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Dipropylcarbamoyl chloride (5.4 g.) was added to a solution of 5.25 g. 3-propylsulphonyl-1,2,4-triazole and 6 ml. dry triethylamine in 25 ml. dry tetrahydrofuran and the resulting mixture was refluxed under anhydrous conditions for 2.5 hours. The cooled reaction mixture was filtered to remove triethylamine hydrochloride, the filtrate was distilled under reduced pressure to remove solvent, and the residue was dissolved in methylene dichloride. The resulting solution was washed with ice-cold 0.1N aqueous sodium hydroxide (2 × 50 ml.), then with 0.01N aqueous sulphuric acid (50 ml.) and finally with water. The resulting solution was dried over anhydrous sodium sulphate and was then distilled under reduced pressure to give a solid residue. This residue was recrystallized twice from petroleum ether (b.p. 60° - 80°C.) to give 1-dipropylcarbamoyl-3-propylsulphonyl-1,2,4-triazole, m.p. 79° - 80°C. Elemental analysis satisfactory.

Aufarbeitung

  1. customThe cooled reaction mixture
  2. filtrationwas filtered
  3. customto remove triethylamine hydrochloride
  4. distillationthe filtrate was distilled under reduced pressure
  5. customto remove solvent
  6. dissolutionthe residue was dissolved in methylene dichloride
  7. washThe resulting solution was washed with ice-cold 0.1N aqueous sodium hydroxide (2 × 50 ml.)
  8. dry with materialThe resulting solution was dried over anhydrous sodium sulphate
  9. distillationwas then distilled under reduced pressure
  10. customto give a solid residue
  11. customThis residue was recrystallized twice from petroleum ether (b.p. 60° - 80°C.)

Quellen und Nachweise

ORD-Eintrag
ord-99415b87f0de42c78bccc59441cf8290
Quelldatensatz
uspto-grants-1976_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US03952001

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