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Trifluoroacetic acid → HCID 136173806, Verbindung

HRID 2079224
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2079224
FC(F)(F)C(O)=O.C(OC(=O)[NH:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[N:21]1[C:25](=[O:26])[NH:24][C:23]([CH:27]([C:41]2[CH:46]=[C:45]([CH2:47][CH3:48])[CH:44]=[C:43]([O:49][CH2:50][C:51](=[O:55])[N:52]([CH3:54])[CH3:53])[C:42]=2[F:56])[NH:28][C:29]2[CH:34]=[CH:33][C:32]([C:35]3[N:39]=[C:38]([CH3:40])[O:37][N:36]=3)=[CH:31][CH:30]=2)=[N:22]1)(C)(C)C>ClCCl>[NH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[N:21]1[C:25](=[O:26])[NH:24][C:23]([CH:27]([NH:28][C:29]2[CH:30]=[CH:31][C:32]([C:35]3[N:39]=[C:38]([CH3:40])[O:37][N:36]=3)=[CH:33][CH:34]=2)[C:41]2[C:42]([F:56])=[C:43]([CH:44]=[C:45]([CH2:47][CH3:48])[CH:46]=2)[O:49][CH2:50][C:51]([N:52]([CH3:54])[CH3:53])=[O:55])=[N:22]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 136173745HCID 136173745, Verbindung

Produkt 1

HCID 136173806HCID 136173806, VerbindungAusbeute 86,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

After adding 2 ml of trifluoroacetic acid to a solution of 0.135 g of [2-(3-{(3-dimethylcarbamoylmethoxy-5-ethyl-2-fluorophenyl)-[4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylamino]methyl}-5-oxo-4,5-dihydro-1H-[1,2,4]triazol-1-yl)phenyl]carbamic acid t-butyl ester in 10 ml of dichloromethane, the reaction mixture was stirred at room temperature for 4 hours, and the solvent was removed under reduced pressure. Next, 50 ml of ethyl acetate and 5 ml of 5% aqueous potassium carbonate were added to the residue, and the organic layer was washed with 20 ml of water and 20 ml of saturated aqueous sodium chloride in that order. The aqueous layer was extracted with 50 ml of ethyl acetate, and then the organic layers were combined and dried over anhydrous magnesium sulfate, the desiccating agent was filtered off and the filtrate was concentrated under reduced pressure. The title compound (0.100 g) was obtained as a white solid.

Aufarbeitung

  1. customthe solvent was removed under reduced pressure
  2. additionNext, 50 ml of ethyl acetate and 5 ml of 5% aqueous potassium carbonate were added to the residue
  3. washthe organic layer was washed with 20 ml of water and 20 ml of saturated aqueous sodium chloride in that order
  4. extractionThe aqueous layer was extracted with 50 ml of ethyl acetate
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationthe desiccating agent was filtered off
  7. concentrationthe filtrate was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-1cf4b835d7f8449bbca78cf6c65caa8b
Quelldatensatz
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07928228B2

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