Dimethylformamide → HCID 66746413, Verbindung

HRID 1175755Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1175755
[C:1]12([CH2:9][CH:8](NC(NC3SC4C=C(F)C=CC=4N=3)=O)[C:7]3[CH:24]=[CH:25][CH:26]=[CH:27][C:6]=3[O:5]1)[CH2:4][CH2:3][CH2:2]2.IC.[C:30](=O)([O-])[O-:31].[K+].[K+].CN(C)C=[O:39]>>[CH3:30][O:31][C:25]1[CH:26]=[CH:27][C:6]2[O:5][C:1]3([CH2:2][CH2:3][CH2:4]3)[CH2:9][C:8](=[O:39])[C:7]=2[CH:24]=1

Komponenten

5

Edukt 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 16123262HCID 16123262, Verbindung

Produkt 1

HCID 66746413HCID 66746413, Verbindung

Versuchsvorschrift

To a solution of 3,4-Dihydro-6-hydroxy-4-oxo-spiro[2H-1-benzopyran-2,1′-cyclobutane] (Example 12) (10 mmol) in dimethylformamide, iodomethane (12 mmol) and potassium carbonate (12 mmol) was added and the reaction mixture was stirred at rt for 12 h. Solvent was then evaporated and the residue was dissolved in ethyl acetate. Organic layer was washed with water, brine and separated. It was then dried on anhydrous Na2SO4 and concentrated to afford the desired product as oil.

Aufarbeitung

  1. customSolvent was then evaporated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washOrganic layer was washed with water, brine
  4. customseparated
  5. dry with materialIt was then dried on anhydrous Na2SO4
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-0b76445fcbd04a59b47089533712d3f0
Quelldatensatz
uspto-grants-2010_11
Patentnummer
US07842703B2

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