Sodium Bicarbonate → HCID 86590125, Verbindung

HRID 1884917Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1884917
[H-].[H-].[H-].[H-].[Li+].[Al+3].[Cl:7][C:8]1[CH:28]=[CH:27][C:26]([Cl:29])=[C:25]([CH3:30])[C:9]=1[C:10]([C:12]1[C:17]([CH3:18])=[CH:16][C:15]([O:19][CH3:20])=[C:14]([O:21][CH3:22])[C:13]=1[O:23][CH3:24])=[O:11].C([O-])(O)=O.[Na+]>O1CCCC1>[Cl:7][C:8]1[CH:28]=[CH:27][C:26]([Cl:29])=[C:25]([CH3:30])[C:9]=1[CH:10]([OH:11])[C:12]1[C:17]([CH3:18])=[CH:16][C:15]([O:19][CH3:20])=[C:14]([O:21][CH3:22])[C:13]=1[O:23][CH3:24]

Komponenten

5

Edukt 3

HCID 516892Sodium BicarbonateHCID 11417330HCID 11417330, VerbindungHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 86590125HCID 86590125, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

Under protective gas conditions, at about −78° C., 1 ml of a 1-molar solution of LiAlH4 in tetrahydrofuran was added dropwise to a solution of 0.37 g of 2,5-dichloro-6,6′-dimethyl-2′, 3′, 4′-trimethoxybenzophenone in 20 ml of anhydrous tetrahydrofuran, and the mixture was stirred for about 1 hour. At 20-25° C., sat. NaHCO3 solution was added to the reaction solution, the solution was extracted with ethyl acetate and the organic phase was washed with water and sat. NaCl solution and dried, and the solvent was then distilled off. The residue gave, after purification by column chromatography (mobile phase: ethyl acetate/cyclohexane 1:9), 150 mg of the title compound as a yellow viscous oil.

Aufarbeitung

  1. extractionthe solution was extracted with ethyl acetate
  2. washthe organic phase was washed with water and sat. NaCl solution
  3. customdried
  4. distillationthe solvent was then distilled off
  5. customThe residue gave
  6. customafter purification by column chromatography (mobile phase: ethyl acetate/cyclohexane 1:9), 150 mg of the title compound as a yellow viscous oil

Quellen und Nachweise

ORD-Eintrag
ord-36847311ec9a451ea48f55015d3839f3
Quelldatensatz
uspto-grants-2004_07
Patentnummer
US06767923B2

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