Dimethylformamide → HCID 66745583, Verbindung

HRID 1175756Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1175756
[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.[CH:28]1(Br)C[CH2:31][CH2:30][CH2:29]1.[C:34]([O-:37])([O-])=O.[K+].[K+].CN(C=[O:44])C>>[CH:34]1([O:37][C:25]2[CH:26]=[CH:27][C:6]3[O:5][C:1]4([CH2:2][CH2:3][CH2:4]4)[CH2:9][C:8](=[O:44])[C:7]=3[CH:24]=2)[CH2:31][CH2:30][CH2:29][CH2:28]1

Komponenten

5

Edukt 4

HCID 6228DimethylformamideHCID 8728BromocyclopentaneHCID 11430Potassium CarbonateHCID 16123262HCID 16123262, Verbindung

Produkt 1

HCID 66745583HCID 66745583, Verbindung

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To a solution of 3,4-Dihydro-6-hydroxy-4-oxo-spiro[2H-1-benzopyran-2,1′-cyclobutane] (from example 12) (10 mmol) in DMF, cyclopentyl bromide (12 mmol) and K2CO3 (12 mmol) was added and the reaction mixture was heated at 60° C. 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-904d19f53f264ff99e7643b27883047b
Quelldatensatz
uspto-grants-2010_11
Patentnummer
US07842703B2

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