Methyl iodide → HCID 19866681, Verbindung

HRID 1199464Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1199464
[CH3:1][S:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[NH:13][C:12]2[CH:14]=[CH:15][CH:16]=[CH:17][C:11]=2[N:10]=1.CI.[C:20](=O)([O-])[O-].[K+].[K+]>CN(C)C=O.[Cl-].[Na+].O>[CH3:20][N:13]1[C:12]2[CH:14]=[CH:15][CH:16]=[CH:17][C:11]=2[N:10]=[C:9]1[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[S:2][CH3:1]

Komponenten

6

Edukt 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 123160831H-Benzimidazole, 2-[2-(methylthio)phenyl]-

Produkt 1

HCID 19866681HCID 19866681, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 57417360Sodium chloride; waterLösungsmittel

Versuchsvorschrift

The product of step (a) above (3.25 g), methyl iodide (1.92 g) and potassium carbonate (5.2 g) were stirred together in dry dimethylformamide (50 ml) at room temperature for 24 hours. The reaction mixture was poured into brine and extracted into ethyl acetate, the extract was washed with excess brine, dried over magnesium sulphate and evaporated to dryness in vacuo and the residue was purified by flash chromatography (SiO2 /CH2Cl2 9:1 ethyl acetate) to afford the sub-title compound as yellow solid, MS MW 254 bp 239.

Aufarbeitung

  1. extractionextracted into ethyl acetate
  2. washthe extract was washed with excess brine
  3. dry with materialdried over magnesium sulphate
  4. customevaporated to dryness in vacuo
  5. customthe residue was purified by flash chromatography (SiO2 /CH2Cl2 9:1 ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-42976fe0c28b40e28a0f396355ff0402
Quelldatensatz
uspto-grants-1990_02
Patentnummer
US04900751

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