Potassium Carbonate → 1-[(Trimethylsilyl)methyl]-4-chloro-3-(2-nitro-3-chlorophenyl)pyrazole

HRID 1376325

Reaktionsgleichung

Reaktionsgleichung von HRID 1376325
C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[C:9]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[C:14]=2[N+:20]([O-:22])=[O:21])=[N:10][NH:11][CH:12]=1.[CH3:23][Si:24]([CH2:27]Cl)([CH3:26])[CH3:25]>CN(C)C=O.CCCCCCC.C(OCC)(=O)C>[CH3:23][Si:24]([CH2:27][N:11]1[CH:12]=[C:8]([Cl:7])[C:9]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[C:14]=2[N+:20]([O-:22])=[O:21])=[N:10]1)([CH3:26])[CH3:25]

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 75361Silane, (chloromethyl)trimethyl-HCID 178526739HCID 178526739, Verbindung

Produkt 1

HCID 229164881-[(Trimethylsilyl)methyl]-4-chloro-3-(2-nitro-3-chlorophenyl)pyrazole

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 21899848Ethylacetate heptaneLösungsmittel

Versuchsvorschrift

0.85 g of anhydrous potassium carbonate is added to a solution of 1.30 g of 4-chloro-3-(2-nitro-3-chlorophenyl)pyrazole and 0.70 g of (trimethylsilyl)methyl chloride in 30 ml of N,N-dimethylformamide. The reaction mixture is stirred for 12 hours at room temperature and diluted with 100 ml of an ether/H2O (1/1) mixture. The ether phase is dried over MgSO4 and concentrated under reduced pressure. The residual oil is purified by liquid chromatography on a Silica column (eluent: heptane/ethyl acetate [50/50]).

Aufarbeitung

  1. dry with materialThe ether phase is dried over MgSO4
  2. concentrationconcentrated under reduced pressure
  3. customThe residual oil is purified by liquid chromatography on a Silica column (eluent: heptane/ethyl acetate [50/50])

Quellen und Nachweise

ORD-Eintrag
ord-8c638eb01e474d6d8a47ec2efe57952c
Quelldatensatz
uspto-grants-1997_09
Patentnummer
US05663119

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