Methanol → HCID 20401795, Verbindung

HRID 1980523Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1980523
[C:1]1([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:6]=[CH:5][C:4]([Si:7]([CH3:12])([CH3:11])[CH:8](Cl)[CH3:9])=[CH:3][CH:2]=1.[K].[NH:20]1[CH:24]=[N:23][CH:22]=[N:21]1.CO>CN(C)C=O.O.ClCCl>[C:1]1([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:6]=[CH:5][C:4]([Si:7]([CH3:12])([CH3:11])[CH:8]([N:20]2[CH:24]=[N:23][CH:22]=[N:21]2)[CH3:9])=[CH:3][CH:2]=1

Komponenten

7

Edukt 3

HCID 887MethanolHCID 20401742HCID 20401742, VerbindungHCID 534465811,2,4-Triazole potassium

Produkt 1

HCID 20401795HCID 20401795, VerbindungAusbeute 13,1 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 2.50 g (7.46 mmol) of 82% pure (1,1'-biphenyl-4-yl)dimethyl-1-chloroethylsilane and 1.60 g (15 mmol) of 1H-1,2,4-triazole potassium salt in 15 ml of dimethylformamide was stirred at 50° for 64 hours, cooled, diluted with water, and extracted with ether. The ether extracts were washed with water and brine, dried over magnesium sulfate, and evaporated to leave a viscous oil. Chromatography over silica gel eluting with 2% methanol in dichloromethane gave 0.30 g (13%) of the title compound as a pale yellow oil: nmr (CDCl3) 0.38 and 0.42 (total 6H, two equal s), 1.6 (3H, d, J=7 Hz), 4.2 (1H, q, J=7 Hz), 7.3-7.8 (9H, m), 7.9 (1H, s) and 8.0 (1H, s).

Aufarbeitung

  1. temperaturecooled
  2. extractionextracted with ether
  3. washThe ether extracts were washed with water and brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated
  6. customto leave a viscous oil

Quellen und Nachweise

ORD-Eintrag
ord-01a983b83e2d4092b650d8a1804ac584
Quelldatensatz
uspto-grants-1985_04
Patentnummer
US04510136

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