Ethyl Acetate → Indane

HRID 36926

Reaktionsgleichung

Reaktionsgleichung von HRID 36926
ClC1C=CC=CC=1C(Cl)=O.N[C:12]1[CH:13]=[C:14]2[C:18](=[CH:19][CH:20]=1)[CH2:17][CH2:16][CH2:15]2.C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C>O>[CH2:17]1[C:18]2[C:14](=[CH:13][CH:12]=[CH:20][CH:19]=2)[CH2:15][CH2:16]1

Komponenten

6

Edukt 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 691102-Chlorobenzoyl chlorideHCID 90496Indan-5-amine

Produkt 1

HCID 10326Indane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

2-Chlorobenzoyl chloride (11.8 g) was added dropwise to a stirred mixture of 5-aminoindan (9.0 g), potassium carbonate (9.3 g), ethyl acetate (90 ml) and water (90 ml) under ice-cooling. The mixture was further stirred under ice-cooling for one hour, at the end of which time the organic layer was separated, washed with water, dried (MgSO4) and distilled to remove the solvent. The procedure gave crystals of 5-2-chlorobenzoylamino)indan. The crystals were collected by filtration and recrystallized from isopropyl ether to give colorless needles, m.p. 144°-145° C.

Aufarbeitung

  1. temperaturecooling
  2. temperaturecooling for one hour, at the end of which time the organic layer
  3. customwas separated
  4. washwashed with water
  5. dry with materialdried (MgSO4)
  6. distillationdistilled
  7. customto remove the solvent

Quellen und Nachweise

ORD-Eintrag
ord-88d69e93a5f6475badf02e8876958cbe
Quelldatensatz
uspto-grants-1995_05
Patentnummer
US05418239

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