((Chloromethyl)phenylethyl)-trimethoxysilane → HCID 178503001, Verbindung

HRID 2103956Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2103956
[SH:1][C:2]1[N:6]=[CH:5][NH:4][N:3]=1.[CH2:7](O[K])C.ClC[CH:13]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[CH2:14][Si:15]([O:20][CH3:21])([O:18][CH3:19])[O:16][CH3:17]>C(O)C>[CH3:21][O:20][Si:15]([O:16][CH3:17])([O:18][CH3:19])[CH2:14][CH2:13][C:22]1[CH:23]=[CH:24][C:25]([CH2:7][S:1][C:2]2[N:6]=[CH:5][NH:4][N:3]=2)=[CH:26][CH:27]=1

Komponenten

5

Edukt 3

HCID 53426825((Chloromethyl)phenylethyl)-trimethoxysilaneHCID 178473702HCID 178473702, VerbindungHCID 178527894HCID 178527894, Verbindung

Produkt 1

HCID 178503001HCID 178503001, VerbindungAusbeute 53 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

10 mmole of 3-mercapto-1H-1,2,4-triazole was dissolved in 20 ml ethanol, then 10 mmole EtOK was added, and stirred for 5 minutes. 10 mmole of ((chloromethyl)phenylethyl)trimethoxysilane was added to the solution, and stirred for 6 hours. The white precipitate was removed by filtration, the solvent in the filtrate was removed in vacuum. The obtained solid was dissolved in methanol, and separated with a Si gel column (solvents: 7 ethylacetate/3 hexane in volume). Yield: 53%. 1H NMR (CDCl3) of Precursors 6: δ(ppm) 8.09 (1H, s), 7.19 (4H, m), 4.29 (2H, s), 3.55 (9H, s), 2.72 (2H, t, JH-H=8.50), 1.02 (2H, t, JH-H=8.50).

Aufarbeitung

  1. stirringstirred for 6 hours
  2. customThe white precipitate was removed by filtration
  3. customthe solvent in the filtrate was removed in vacuum
  4. dissolutionThe obtained solid was dissolved in methanol
  5. customseparated with a Si gel column (solvents: 7 ethylacetate/3 hexane in volume)

Quellen und Nachweise

ORD-Eintrag
ord-14288d0c3f00407286a109f65d1ae6f4
Quelldatensatz
uspto-grants-2009_08
Patentnummer
US07576165B2

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