Acetone → HCID 57419464, Verbindung

HRID 1962319

Reaktionsgleichung

Reaktionsgleichung von HRID 1962319
O[C:2]1[C:10]([I:11])=[CH:9][C:8]([I:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S([O:18][CH3:19])(OC)(=O)=O.[CH3:20]C(C)=O>>[I:11][C:10]1[C:2]([O:18][CH3:19])=[C:3]([CH:7]=[C:8]([I:12])[CH:9]=1)[C:4]([O:6][CH3:20])=[O:5]

Komponenten

4

Edukt 3

HCID 180AcetoneHCID 6497Dimethyl SulfateHCID 86313,5-Diiodosalicylic acid

Produkt 1

HCID 57419464HCID 57419464, Verbindung

Versuchsvorschrift

A mixture of 2-hydroxy-3,5-diiodobenzoic acid (3.9 g, 10.0 mmol) potassium carbonate (4.15 g, 30.0 mmol) and dimethyl sulfate (2.77 g, 22.0 mmol) in acetone (33 ml) was heated at reflux for 16 h, cooled and concentrated. The residue was dissolved in EtOAc and washed with water, brine, dried (Na2SO4), filtered and concentrated to give an off-white solid (4.2 g, quantitative yield).

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux for 16 h
  3. temperaturecooled
  4. concentrationconcentrated
  5. dissolutionThe residue was dissolved in EtOAc
  6. washwashed with water, brine
  7. dry with materialdried (Na2SO4)
  8. filtrationfiltered
  9. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-f2eee1525b204e288b52bcb181a85185
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08415351B2

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