4-(4-Fluoro-benzyloxy)-phthalic acid bis-(4-fluoro-benzyl) ester → 4-(4-Fluoro-benzyloxy)-phthalic acid

HRID 1070679Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1070679
FC1C=CC(C[O:7][C:8](=[O:35])[C:9]2[C:10](=[CH:22][C:23]([O:26][CH2:27][C:28]3[CH:33]=[CH:32][C:31]([F:34])=[CH:30][CH:29]=3)=[CH:24][CH:25]=2)[C:11]([O:13]CC2C=CC(F)=CC=2)=[O:12])=CC=1>O1CCCC1.O>[F:34][C:31]1[CH:30]=[CH:29][C:28]([CH2:27][O:26][C:23]2[CH:22]=[C:10]([C:11]([OH:13])=[O:12])[C:9](=[CH:25][CH:24]=2)[C:8]([OH:35])=[O:7])=[CH:33][CH:32]=1

Komponenten

4

Edukt 1

HCID 697368654-(4-Fluoro-benzyloxy)-phthalic acid bis-(4-fluoro-benzyl) ester

Produkt 1

HCID 223970954-(4-Fluoro-benzyloxy)-phthalic acidAusbeute 56 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A mixture of 4-(4-fluoro-benzyloxy)-phthalic acid bis-(4-fluoro-benzyl) ester (7.8 g, 15.4 mmol) lithium hydroxide monohydrate (1.8 g, 46.2 mmol) in tetrahydrofuran (60 mL) and water (60 mL) was stirred at room temperature for 72 h. The mixture was then evaporated followed by acidification to pH 2 at 0° C. with concentrated HCl. The organic layer was then diluted with ethyl acetate, separared, washed with water and dried over sodium sulfate. Filtration and half evaporation gave a white suspension which was filtered off and washed with ether to afford the title compound (2.5 g, 56%) as a white solid.

Aufarbeitung

  1. customThe mixture was then evaporated
  2. customfollowed by acidification to pH 2 at 0° C. with concentrated HCl
  3. additionThe organic layer was then diluted with ethyl acetate
  4. washwashed with water
  5. dry with materialdried over sodium sulfate
  6. filtrationFiltration and half evaporation
  7. customgave a white suspension which
  8. filtrationwas filtered off
  9. washwashed with ether

Quellen und Nachweise

ORD-Eintrag
ord-bd24580e823649e9b37825c97ec4df82
Quelldatensatz
uspto-grants-2005_06
Patentnummer
US06903095B2

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