Sodium Iodide → 84422-52-6

HRID 493208

Reaktionsgleichung

Reaktionsgleichung von HRID 493208
C[O:2][C:3]1[CH:10]=[C:9]([O:11][CH3:12])[C:8]([CH3:13])=[CH:7][C:4]=1[CH:5]=[O:6].[I-].[Na+].[Al+3].[Cl-].[Cl-].[Cl-]>C(#N)C>[OH:2][C:3]1[CH:10]=[C:9]([O:11][CH3:12])[C:8]([CH3:13])=[CH:7][C:4]=1[CH:5]=[O:6]

Komponenten

5

Edukt 3

HCID 5238Sodium IodideHCID 2516922,4-Dimethoxy-5-methylbenzaldehydeHCID 6451240Aluminum(III) Chloride

Produkt 1

HCID 1316681984422-52-6

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

The above prepared 2,4-Dimethoxy-5-methyl-benzaldehyde (5.40 g, 30 mmol) was dissolved in 150 mL of acetonitrile and treated successively with sodium iodide (6.74 g, 1.5 eq.) and AlCl3 (4.00 g, 1.0 eq.), and the mixture kept at 80° C. for 1 h. Cooling, pouring onto crashed ice, twofold extraction with AcOEt, washing with water and brine, drying over magnesium sulfate, and evaporation of the solvents, followed by flash chromatography (SiO2, hexane/AcOEt=9/1), delivered 4.23 g of the title compound as light brown crystals.

Aufarbeitung

  1. temperatureCooling
  2. additionpouring
  3. extractionice, twofold extraction with AcOEt
  4. washwashing with water and brine
  5. dry with materialdrying over magnesium sulfate, and evaporation of the solvents

Quellen und Nachweise

ORD-Eintrag
ord-11a5a2acbeae4b778a041cb41b2954dc
Quelldatensatz
uspto-grants-2009_05
Patentnummer
US07534788B2

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