7-dimethylamino-6,7-dihydro [5H] benzocycloheptene → HCID 3046863, Verbindung

HRID 372542Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 372542
[CH3:1][N:2]([CH3:14])[CH:3]1[CH:9]=[CH:8][C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[CH2:5][CH2:4]1>C(O)C>[CH3:1][N:2]([CH3:14])[CH:3]1[CH2:9][CH2:8][C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[CH2:5][CH2:4]1

Komponenten

3

Edukt 1

HCID 30468617-dimethylamino-6,7-dihydro [5H] benzocycloheptene

Produkt 1

HCID 3046863HCID 3046863, VerbindungAusbeute 36,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 11.2 g of 7-dimethylamino-6,7-dihydro [5H] benzocycloheptene, 800 ml of ethanol and 11.2 g carbon containing 10% of Pd (OH)2 was held under a hydrogen atmosphere for 30 minutes and when the theoretical amount of hydrogen had been absorbed, the mixture was filtered. The filtrate was evaporated to dryness and the residue was chromatographed over silica gel. Elution with an 8-2-1 ethyl acetate-benzene-triethylamine mixture yielded 4.1 g of 7-dimethylamino-6,7,8,9-tetrahydro [5H] benzocycloheptene.

Aufarbeitung

  1. customwhen the theoretical amount of hydrogen had been absorbed
  2. filtrationthe mixture was filtered
  3. customThe filtrate was evaporated to dryness
  4. customthe residue was chromatographed over silica gel
  5. washElution with an 8-2-1 ethyl acetate-benzene-triethylamine mixture

Quellen und Nachweise

ORD-Eintrag
ord-67190c1bc9fe4862a4af33c88bc1dd26
Quelldatensatz
uspto-grants-1978_05
Patentnummer
US04091115

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