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Lawesson's reagent → 6,11-Dihydro-N-(2,6-diisopropylphenyl)-2-methyldibenz[b,e]oxepin-11-carbothioamide

HRID 2260590
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2260590
[CH:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH:10]([CH3:12])[CH3:11])[C:5]=1[NH:13][C:14]([CH:16]1[C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=2[CH2:20][O:19][C:18]2[CH:27]=[CH:28][C:29]([CH3:31])=[CH:30][C:17]1=2)=O)([CH3:3])[CH3:2].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:41])=CC=1>C1(C)C=CC=CC=1>[CH:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH:10]([CH3:12])[CH3:11])[C:5]=1[NH:13][C:14]([CH:16]1[C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=2[CH2:20][O:19][C:18]2[CH:27]=[CH:28][C:29]([CH3:31])=[CH:30][C:17]1=2)=[S:41])([CH3:3])[CH3:2]
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Komponenten

4

Edukt 2

HCID 87949Lawesson's reagentHCID 3072807Dibenz(b,e)oxepin-11-carboxamide, 6,11-dihydro-N-(2,6-bis(1-methylethyl)phenyl)-2-methyl-

Produkt 1

HCID 104553336,11-Dihydro-N-(2,6-diisopropylphenyl)-2-methyldibenz[b,e]oxepin-11-carbothioamideAusbeute 96,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

After 1.09 g of Compound 4 obtained in Example 4 was dissolved in 10 ml of toluene, 1.07 g of Lawesson's reagent was added to the solution. The mixture was heated under reflux for an hour. The reaction mixture was allowed to stand at room temperature, and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography [eluent: hexane-ethyl acetate (2:1)] to obtain 1.46 g of a crude product. The crude product was recrystallized from ethyl acetate-hexane to obtain 1.09 g of Compound 36.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for an hour
  3. customto stand at room temperature
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting residue was purified by silica gel column chromatography [eluent: hexane-ethyl acetate (2:1)]
  6. customto obtain 1.46 g of a crude product
  7. customThe crude product was recrystallized from ethyl acetate-hexane

Quellen und Nachweise

ORD-Eintrag
ord-ab9b161e45c343ca9daa8c8693bf846c
Quelldatensatz
uspto-grants-1995_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05478835

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