HCID 58629740, Verbindung → HCID 58629777, Verbindung

HRID 423261Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 423261
[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:9]=[C:8]([O:10][CH3:11])[C:7]([O:12][CH2:13][O:14][CH3:15])=[C:6](I)[CH:5]=1.[CH3:18][Zn]C.C1COCC1>C1COCC1.C(OCC)(=O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:5]=[C:6]([CH3:18])[C:7]([O:12][CH2:13][O:14][CH3:15])=[C:8]([O:10][CH3:11])[CH:9]=1

Komponenten

6

Edukt 2

HCID 58629740HCID 58629740, VerbindungHCID 178420677HCID 178420677, Verbindung

Produkt 1

HCID 58629777HCID 58629777, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 178418397HCID 178418397, VerbindungKatalysatorHCID 8028TetrahydrofuranLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To a solution of 3-iodo-5-methoxy-4-methoxymethoxybenzoic acid methyl ester (700 mg) in THF (7 mL) were added tetrakis(triphenylphosphine)palladium(0) (115 mg) and 2M dimethylzinc/THF solution (1.20 mL), and the mixture was stirred at 80° C. for 30 minutes. The reaction solution was diluted with ethyl acetate, washed with 1N hydrochloric acid, water, and saturated brine, dried over anhydrous sodium sulfate, and concentrated in vacuo to give the title compound (767 mg) as a crude purified product of pale yellow oil.

Aufarbeitung

  1. washwashed with 1N hydrochloric acid, water, and saturated brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-7b12c58f793d4e59befb3ec9ed4bc0ea
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08101774B2

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