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Ethyl Acetate → HCID 72312772, Verbindung

HRID 2079221
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2079221
C(=O)([O-])[O-].[K+].[K+].Cl[CH2:8][C:9]([N:11]([CH3:13])[CH3:12])=[O:10].[CH3:14][O:15][C:16](=[O:45])[N:17]=[C:18]([S:43][CH3:44])[C:19]([C:33]1[CH:38]=[C:37]([CH2:39][CH3:40])[CH:36]=[C:35]([OH:41])[C:34]=1[F:42])=[N:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]2[N:31]=[C:30]([CH3:32])[O:29][N:28]=2)=[CH:23][CH:22]=1.C(OCC)(=O)C>CN(C=O)C.O>[CH3:14][O:15][C:16](=[O:45])[N:17]=[C:18]([S:43][CH3:44])[C:19]([C:33]1[CH:38]=[C:37]([CH2:39][CH3:40])[CH:36]=[C:35]([O:41][CH2:8][C:9](=[O:10])[N:11]([CH3:13])[CH3:12])[C:34]=1[F:42])=[N:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]2[N:31]=[C:30]([CH3:32])[O:29][N:28]=2)=[CH:23][CH:22]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 758862-chloro-N,N-dimethylacetamideHCID 72312790HCID 72312790, Verbindung

Produkt 1

HCID 72312772HCID 72312772, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962
Water
Lösungsmittel
HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

After adding 0.163 g of potassium carbonate and 0.14 ml of 2-chloro-N, N-dimethylacetamide to a solution of 0.41 g of {2-(5-ethyl-2-fluoro-3-hydroxyphenyl)-2-[4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylimino]-1-methylsulfanylethylidene}carbamic acid methyl ester in 15 ml of DMF, the reaction mixture was stirred at room temperature for 60 hours, and then 200 ml of ethyl acetate and 100 ml of water were added. The organic layer was washed twice with 100 ml of water and once with 100 ml of saturated aqueous sodium chloride in that order, and dried over anhydrous magnesium sulfate. The desiccating agent was filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate-heptane) to give the title compound (0.41 g) as a light yellow solid.

Aufarbeitung

  1. washThe organic layer was washed twice with 100 ml of water and once with 100 ml of saturated aqueous sodium chloride in that order
  2. dry with materialdried over anhydrous magnesium sulfate
  3. filtrationThe desiccating agent was filtered
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (ethyl acetate-heptane)

Quellen und Nachweise

ORD-Eintrag
ord-834a8d0b6a834091bc7953fc23de1ee2
Quelldatensatz
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07928228B2

Notizen zur Reaktion

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