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Sodium Hydroxide → HCID 69357330, Verbindung

HRID 852544
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 852544
[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:13]=[C:12]([O:14][CH2:15][CH3:16])[CH:11]=[C:6]([C:7]([O:9]C)=[O:8])[CH:5]=1.[OH-].[Na+]>CO>[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:13]=[C:12]([O:14][CH2:15][CH3:16])[CH:11]=[C:6]([C:7]([OH:9])=[O:8])[CH:5]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 68538880HCID 68538880, Verbindung

Produkt 1

HCID 69357330HCID 69357330, VerbindungAusbeute 82,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of 5-ethoxy-isophthalic acid dimethyl ester (D43) (22 g, 92.4 mmol, 1 equiv) in MeOH (440 ml) was added 1N aqueous NaOH solution (87.8 ml, 87.8 mmol, 0.95 equiv) and the resulting solution was stirred at room temperature for 17 h. Most of the MeOH was removed in vacuo and the residue was partitioned between AcOEt and 1N aqueous NaOH solution. The aqueous layer was extracted with AcOEt, acidified to pH 1 and re-extracted with AcOEt. The second organic extract was dried over MgSO4 and concentrated in vacuo to give 5-ethoxy-isophthalic acid monomethyl ester (D45) (17 g, 82%) as a white solid. [M+H+ NH3]+=242.0, RT=2.79 min

Aufarbeitung

  1. customMost of the MeOH was removed in vacuo
  2. customthe residue was partitioned between AcOEt and 1N aqueous NaOH solution
  3. extractionThe aqueous layer was extracted with AcOEt
  4. extractionre-extracted with AcOEt
  5. extractionThe second organic extract
  6. dry with materialwas dried over MgSO4
  7. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-78fa2a39409a4fab9a8b2293e0d49f36
Quelldatensatz
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07253198B2

Notizen zur Reaktion

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