Lithium Hydroxide → 2-Indancarboxylic Acid

HRID 37377

Reaktionsgleichung

Reaktionsgleichung von HRID 37377
[C:1]([C:6]1(C(OCC)=O)[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7]1)([O:3]CC)=[O:2].[OH-].[Li+]>C(O)C>[C:1]([CH:6]1[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7]1)([OH:3])=[O:2]

Komponenten

4

Edukt 2

HCID 3939Lithium HydroxideHCID 110107772,2-Dicarboethoxy-indane

Produkt 1

HCID 5757772-Indancarboxylic AcidAusbeute 71 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Dissolve 2,2-dicarboethoxy-indan (5.67 g, 21.7 mmol) in ethanol (150 mL). Add 1N lithium hydroxide (50 mL) and stir overnight at room temperature. Reflux for 1 hour and concentrate the solution in vacuo. Partition between ethyl acetate and 6N hydrochloric acid. Separate the organic phase and wash with brine. Dry (MgSO4) and evaporate the solvent i n vacuo to give an off-white solid. Distill (120°-160° C. @0 .2-0.5 mmHg) to give 2-carboxy-indan (2.5 g, 71%).

Aufarbeitung

  1. temperatureReflux for 1 hour
  2. concentrationconcentrate the solution in vacuo
  3. customPartition between ethyl acetate and 6N hydrochloric acid
  4. customSeparate the organic phase
  5. washwash with brine
  6. dry with materialDry (MgSO4)
  7. customevaporate the solvent i n vacuo
  8. customto give an off-white solid
  9. distillationDistill (120°-160° C. @0 .2-0.5 mmHg)

Quellen und Nachweise

ORD-Eintrag
ord-925e6b2b9f4843428e1f54535f85a285
Quelldatensatz
uspto-grants-1995_05
Patentnummer
US05420271

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