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Potassium Carbonate → HCID 22938523, Verbindung

HRID 856715
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 856715
[NH:1]1[CH:5]=[C:4]([C:6]([O:8][CH3:9])=[O:7])[N:3]=[N:2]1.C(=O)([O-])[O-].[K+].[K+].I[CH2:17][CH2:18][CH3:19]>CN(C=O)C>[CH2:17]([N:2]1[N:3]=[C:4]([C:6]([O:8][CH3:9])=[O:7])[CH:5]=[N:1]1)[CH2:18][CH3:19].[CH2:17]([N:1]1[CH:5]=[C:4]([C:6]([O:8][CH3:9])=[O:7])[N:3]=[N:2]1)[CH2:18][CH3:19]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 336431-IodopropaneHCID 178498891HCID 178498891, Verbindung

Produkt 2

HCID 22938523HCID 22938523, VerbindungHCID 22938529Methyl 1-propyl-1H-1,2,3-triazole-4-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228
Dimethylformamide
Lösungsmittel

Versuchsvorschrift

methyl 1,2,3-triazole-4-carboxylate (17.6 g) was dissolved in DMF (210 ml), potassium carbonate (11.5 g) and iodopropane (14.9 ml) were added to the mixture, and the mixture was stirred for 16 hours at room temperature. After filtration, the solvent was removed under reduced pressure, and water was added to the obtained residue, and the mixture was extracted with methylene chloride. The organic layer was washed with saturated brine, and dried over magnesium sulfate. The solvent was removed under reduced pressure, and the obtained residue was purified by silica gel column chromatography, to give methyl 2-propyl-1,2,3-triazole-4-carboxylate (10.3 g), methyl 1-propyl-1,2,3-triazole-5-carbonate (3.2 g) and methyl 1-propyl-1,2,3-triazole-4-carboxylate (2.6 g).

Aufarbeitung

  1. filtrationAfter filtration
  2. customthe solvent was removed under reduced pressure, and water
  3. additionwas added to the obtained residue
  4. extractionthe mixture was extracted with methylene chloride
  5. washThe organic layer was washed with saturated brine
  6. dry with materialdried over magnesium sulfate
  7. customThe solvent was removed under reduced pressure
  8. customthe obtained residue was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-f706a72bc4dc42e98b2ebc9ee97c53fa
Quelldatensatz
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07262185B2

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