1,2-Bis(2-iodoethoxy)ethane → 1,2-bis(2-(3H-1,2,3-triazol-4-ylthio)ethoxy)ethane

HRID 2103944Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2103944
I[CH2:2][CH2:3][O:4][CH2:5][CH2:6][O:7][CH2:8][CH2:9]I.[SH:11][C:12]1[NH:16][N:15]=[N:14][CH:13]=1>C(O)C>[N:14]1[CH:13]=[C:12]([S:11][CH2:2][CH2:3][O:4][CH2:5][CH2:6][O:7][CH2:8][CH2:9][S:11][C:12]2[NH:16][N:15]=[N:14][CH:13]=2)[NH:16][N:15]=1

Komponenten

4

Edukt 2

HCID 5934361,2-Bis(2-iodoethoxy)ethaneHCID 178527741HCID 178527741, Verbindung

Produkt 1

HCID 1784209301,2-bis(2-(3H-1,2,3-triazol-4-ylthio)ethoxy)ethaneAusbeute 88 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

10 ml of 1,2-bis(2-iodoethoxy)-ethane was dropped into the solution of 20 mmole 5-mercapto-1H-1,2,3-triazole (sodium salt) in 20 ml ethanol, and stirred for 24 hours at room temperature. After the solvent was evaporated in vacuum, the residual was separated with silica gel column. Elution with hexane/ethylacetate (1/3) first, and then with pure ethyl acetate gave 2.70 g product as viscous solid. Yield: 88%. 1H NMR (CDCl3): δ(ppm) 7.72 (2H, s), 3.74 (4H, t, JH-H=6.19), 3.65 (4H, s), 3.07 (4H, t, JH-H=6.19).

Aufarbeitung

  1. customAfter the solvent was evaporated in vacuum
  2. customthe residual was separated with silica gel column
  3. washElution with hexane/ethylacetate (1/3) first

Quellen und Nachweise

ORD-Eintrag
ord-daa5aa3cc4414293803f006ab10e6f03
Quelldatensatz
uspto-grants-2009_08
Patentnummer
US07576165B2

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