Acetone → HCID 57419464, Verbindung

HRID 2280599

Reaktionsgleichung

Reaktionsgleichung von HRID 2280599
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-cfbddf66c38f4181be7b0e49b7c128a7
Quelldatensatz
uspto-grants-2015_09
Patentnummer
US09139536B2

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