Succinic anhydride → Succinic acid Fluorenylmethyl Ester

HRID 634991

Reaktionsgleichung

Reaktionsgleichung von HRID 634991
[C:1]1([CH2:14][OH:15])[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[C:16]1(=[O:22])[O:21][C:19](=[O:20])[CH2:18][CH2:17]1>C(Cl)Cl>[C:1]1([CH2:14][O:15][C:16](=[O:22])[CH2:17][CH2:18][C:19]([OH:21])=[O:20])[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1

Komponenten

4

Edukt 2

HCID 7922Succinic anhydride2×HCID 523071-Fluorenemethanol

Produkt 1

HCID 69916676Succinic acid Fluorenylmethyl Ester

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Fluorenemethanol (10.0 g, 51.0 mmol) was dissolved in 150 ml CH2Cl2, and succinic anhydride (5.6 g, 56 mmol) was added. The solution was stirred for 6 h, and a further portion of succinic anhydride (2.5 g, 25 mmol) was added, and stirring continued overnight. The reaction appeared complete by TLC. The solvent was then removed, and the residue extracted with ethyl acetate, washed with 1% HCl, water, brine, dried (MgSO4) and evaporated to an oil which crystallized on standing. A quantitative yield of crude product was obtained which was used without further purification.

Aufarbeitung

  1. stirringstirring continued overnight
  2. customThe solvent was then removed
  3. extractionthe residue extracted with ethyl acetate
  4. washwashed with 1% HCl, water, brine
  5. dry with materialdried (MgSO4)
  6. customevaporated to an oil which
  7. customcrystallized on standing

Quellen und Nachweise

ORD-Eintrag
ord-64843d96446146ccb080137976478364
Quelldatensatz
uspto-grants-2001_02
Patentnummer
US06184389B2

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