Tributyltin Chloride → HCID 178440077, Verbindung

HRID 252614Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 252614
[CH2:1]([O:3][C:4]([C:6]1[N:10]([CH2:11][C:12]2[CH:17]=[CH:16][C:15]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[C:24]#[N:25])=[CH:14][CH:13]=2)[C:9]([CH2:26][CH2:27][CH3:28])=[N:8][C:7]=1[C:29]([OH:32])([CH3:31])[CH3:30])=[O:5])[CH3:2].C([Sn](Cl)(CCCC)CCCC)CCC.[N-:47]=[N+:48]=[N-:49].[Na+]>C1(C)C=CC=CC=1>[CH2:1]([O:3][C:4]([C:6]1[N:10]([CH2:11][C:12]2[CH:17]=[CH:16][C:15]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[C:24]3[NH:49][N:48]=[N:47][N:25]=3)=[CH:14][CH:13]=2)[C:9]([CH2:26][CH2:27][CH3:28])=[N:8][C:7]=1[C:29]([OH:32])([CH3:30])[CH3:31])=[O:5])[CH3:2]

Komponenten

5

Edukt 3

HCID 15096Tributyltin ChlorideHCID 33557Sodium AzideHCID 15461993Ethyl 1-((2'-cyano(1,1'-biphenyl)-4-yl)methyl)-4-(1-hydroxy-1-methylethyl)-2-propyl-1H-imidazole-5-carboxylate

Produkt 1

HCID 178440077HCID 178440077, VerbindungAusbeute 134,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

The mixture of 0.56 g (0.8 mmol) ethyl-4-(1-hydroxy-1-methylethyl)-2-propyl-1-[(2′-cyanobiphenyl-4-yl)-methyl]-imidazole-5-carboxylate, 3 ml toluene, 0.65 ml (2.1 mmol) tributyltin chloride and 0.13 mg (2 mmol) NaN3, were heated under reflux for 42 h. The reaction mixture was evaporated under reduced pressure and the residue was dissolved in 5.5 ml of 2.5 M HCl in ethanol. The solution was stirred for 18 h and then concentrated. The residue was triturated in diisopropyl ether to give 0.51 g of the title compound as hydrochloride salt.

Aufarbeitung

  1. temperaturewere heated
  2. temperatureunder reflux for 42 h
  3. customThe reaction mixture was evaporated under reduced pressure
  4. dissolutionthe residue was dissolved in 5.5 ml of 2.5 M HCl in ethanol
  5. concentrationconcentrated
  6. customThe residue was triturated in diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-e1aae7dad1ed406484943c2d74c11e60
Quelldatensatz
uspto-grants-2011_01
Patentnummer
US07868180B2

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