4-Phenyl-3,4-dihydro-1H-benzo[h]quinolin-2-one → HCID 66818900, Verbindung

HRID 2092358Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2092358
[C:1]1([CH:7]2[C:16]3[C:11](=[C:12]4[CH:20]=[CH:19][CH:18]=[CH:17][C:13]4=[CH:14][CH:15]=3)[NH:10][C:9](=[O:21])[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[S]>C(O)(=O)C>[C:1]1([C:7]2[C:16]3[C:11](=[C:12]4[CH:20]=[CH:19][CH:18]=[CH:17][C:13]4=[CH:14][CH:15]=3)[NH:10][C:9](=[O:21])[CH:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Komponenten

4

Edukt 2

HCID 28297134-Phenyl-3,4-dihydro-1H-benzo[h]quinolin-2-oneHCID 5362487Sulfur2×

Produkt 1

HCID 66818900HCID 66818900, VerbindungAusbeute 15 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
205 °C

Versuchsvorschrift

A mixture of 4-Phenyl-3,4-dihydro-1H-benzo[h]quinolin-2-one (0.55 g, 2.0 mmol) and sulfur (0.06 g, 2 mmol) was stirred at 205° C. for 0.5 hr under a nitrogen atmosphere. A second batch of sulfur (0.06 g, 2 mmol) was added and the solution stirred for 12 hr at 205° C. The product was dissolved in hot acetic acid and filtered. The clear filtrate upon cooling deposited crystals that were separated by filtration and washed with acetic acid and water followed by vacuum drying to afford the title compound (0.08 g, 0.30 mmol).

Aufarbeitung

  1. stirringthe solution stirred for 12 hr at 205° C
  2. filtrationfiltered
  3. temperatureThe clear filtrate upon cooling
  4. customwere separated by filtration
  5. washwashed with acetic acid and water
  6. customdrying

Quellen und Nachweise

ORD-Eintrag
ord-35728be90a21446bb156cd7de36402ed
Quelldatensatz
uspto-grants-2013_05
Patentnummer
US08440705B2

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