Aluminum(III) Chloride → HCID 12395586, Verbindung

HRID 1283251Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1283251
[CH3:1][C:2]1([CH:16]([CH3:18])[CH3:17])[CH2:10][C:9]2[C:4](=[C:5]([Cl:14])[C:6]([Cl:13])=[C:7]([O:11]C)[CH:8]=2)[C:3]1=[O:15].[Cl-].[Al+3].[Cl-].[Cl-]>CCCCCCC>[CH3:1][C:2]1([CH:16]([CH3:18])[CH3:17])[CH2:10][C:9]2[C:4](=[C:5]([Cl:14])[C:6]([Cl:13])=[C:7]([OH:11])[CH:8]=2)[C:3]1=[O:15]

Komponenten

4

Edukt 2

HCID 6451240Aluminum(III) ChlorideHCID 12395564HCID 12395564, Verbindung

Produkt 1

HCID 12395586HCID 12395586, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8900HeptaneLösungsmittel

Versuchsvorschrift

A stirred suspension of 2-methyl-2-isopropyl-5-methoxy-6,7-dichloro-1-indanone (7.0 g., 0.0244 mole) and aluminum chloride (9.0 g., 0.068 mole) in heptane (400 ml.) is refluxed for 1 hour and cooled. The heptane is decanted from the reaction mixture and the solid residue is poured into water (300 ml.) and concentrated hydrochloric acid (20 ml.). The crude product is extracted into ether (300 ml.), washed with water, dried over magnesium sulfate, distilled to a volume of 100 ml. and treated with hexane (100 ml.). The 2-methyl-2-isopropyl-5-hydroxy-6,7-dichloro-1-indanone which separates (6.5 g.) melts at 215°C.

Aufarbeitung

  1. temperatureis refluxed for 1 hour
  2. temperaturecooled
  3. customThe heptane is decanted from the reaction mixture
  4. additionthe solid residue is poured into water (300 ml.) and concentrated hydrochloric acid (20 ml.)
  5. extractionThe crude product is extracted into ether (300 ml.)
  6. washwashed with water
  7. dry with materialdried over magnesium sulfate
  8. distillationdistilled to a volume of 100 ml
  9. additionand treated with hexane (100 ml.)

Quellen und Nachweise

ORD-Eintrag
ord-6b7d67fafc524922a3c9b4af2de1fed0
Quelldatensatz
uspto-grants-1976_08
Patentnummer
US03974212

Notizen zur Reaktion

Wird geladen…