Hydrochloric Acid → 1-Benzyl-2-methyl-1,4,5,6-tetrahydro-1,3,6-triaza-benzo[e]azulene

HRID 220784Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 220784
[CH2:1]([N:8]1[C:17]2[C:16]3[CH:18]=[CH:19][CH:20]=[CH:21][C:15]=3[N:14](C(C3C=CC=CC=3)=O)[CH2:13][CH2:12][C:11]=2[N:10]=[C:9]1[CH3:30])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl>CO>[CH2:1]([N:8]1[C:17]2[C:16]3[CH:18]=[CH:19][CH:20]=[CH:21][C:15]=3[NH:14][CH2:13][CH2:12][C:11]=2[N:10]=[C:9]1[CH3:30])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 57555380(1-Benzyl-2-methyl-4,5-dihydro-1H-1,3,6-triaza-benzo[e]azulen-6-yl)-phenyl-methanone

Produkt 1

HCID 575554001-Benzyl-2-methyl-1,4,5,6-tetrahydro-1,3,6-triaza-benzo[e]azuleneAusbeute 78 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

(1-Benzyl-2-methyl-4,5-dihydro-1H-1,3,6-triaza-benzo[e]azulen-6-yl)-phenyl-methanone from Example E5a.1 (5.73 g, 14.6 mmol) was placed in methanol (50 ml) and a 6M HCl aqueous solution (200 ml) was added. The reaction mixture was heated at reflux for 18 h then concentrated in vacuo. The residue was dissolved in dichloromethane, basified with saturated NaHCO3 then washed with brine, dried and concentrated in vacuo to yield the title compound (3.30 g, 78%).

Aufarbeitung

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 18 h
  3. concentrationthen concentrated in vacuo
  4. dissolutionThe residue was dissolved in dichloromethane
  5. washthen washed with brine
  6. customdried
  7. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-8d1cb204aea94ec686d6fbc7019208dc
Quelldatensatz
uspto-grants-2012_06
Patentnummer
US08202858B2

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