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Sodium Thiosulfate → HCID 22938707, Verbindung

HRID 856716
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 856716
[H-].[Li+].[Al+3].[H-].[H-].[H-].[CH2:7]([N:10]1[N:14]=[C:13]([C:15](OC)=[O:16])[CH:12]=[N:11]1)[CH2:8][CH3:9].S([O-])([O-])(=O)=S.[Na+].[Na+]>C1COCC1>[OH:16][CH2:15][C:13]1[CH:12]=[N:11][N:10]([CH2:7][CH2:8][CH3:9])[N:14]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 24477Sodium ThiosulfateHCID 21226445Aluminium lithium hydrideHCID 22938523HCID 22938523, Verbindung

Produkt 1

HCID 22938707HCID 22938707, VerbindungAusbeute 101 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a solution of aluminum lithium hydride (1.57 g) in THF (140 ml) was added dropwise methyl 2-propyl-1,2,3-triazole-4-carboxylate (7.0 g) in. THF (70 ml) at 0° C. The mixture was stirred for 1 hour at room temperature, and an aqueous solution of saturated sodium thiosulfate was added to the mixture at 0° C. The mixture was filtered with Celite, and washed with ethanol. The solvent was removed under reduced pressure, and the obtained residue was purified by silica gel column chromatography, to give 4-hydroxymethyl-2-propyl-1,2,3-triazole (5.9 g). To 4-hydroxymethyl-2-propyl-1,2,3-triazole (4.0 g), thionyl chloride (32 ml) was added to the mixture at 0° C., and the mixture was heated to reflux for 1 hour. After allowing the mixture to be cooled to room temperature, the solvent was removed under reduced pressure, to give 4-chloromethyl-2-propyl-1,2,3-triazole (4.2 g).

Aufarbeitung

  1. customat 0° C
  2. filtrationThe mixture was filtered with Celite
  3. washwashed with ethanol
  4. customThe solvent was removed under reduced pressure
  5. customthe obtained residue was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-c8de837da4ec495ab2ac298eceb9758d
Quelldatensatz
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07262185B2

Notizen zur Reaktion

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