Lawesson's reagent → HCID 18992239, Verbindung

HRID 375616Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 375616
[CH3:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=O)[N:7]3[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][C:8]3=[N:9]2)=[CH:4][CH:3]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:27])=CC=1>C1(C)C=CC=CC=1>[CH3:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[S:27])[N:7]3[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][C:8]3=[N:9]2)=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 87949Lawesson's reagentHCID 139119483-Methyl-7,8,9,10-tetrahydroazepino[2,1-b]quinazolin-12(6H)-one

Produkt 1

HCID 18992239HCID 18992239, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

9 g of 3-methyl-6,7,8,9,10,12-hexahydroazepino[2,1-b]quinazolin-12-one was treated with 15 g of Lawesson's reagent in toluene at reflux under nitrogen until the starting material was consumed, checked by TLC, using chloroform as eluent (24 hours). The mixture was concentrated in vacuo and chromatographed on silica gel, using chloroform as eluent. The bright yellow material was recrystallized from hexane-ethyl acetate.

Aufarbeitung

  1. temperatureat reflux under nitrogen until the starting material
  2. customwas consumed
  3. custom(24 hours)
  4. concentrationThe mixture was concentrated in vacuo
  5. customchromatographed on silica gel
  6. customThe bright yellow material was recrystallized from hexane-ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-154dedbd85924c5c9e7fb377657d0cc0
Quelldatensatz
uspto-grants-1996_01
Patentnummer
US05486512

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