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Sodium Hydroxide → HCID 22228131, Verbindung

HRID 1744588
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1744588
C([CH:3]([C:38]([OH:40])=[O:39])[N:4]([C:19]([C:21]1[C:22]([CH3:37])=[N:23][N:24]([C:26]2[CH:31]=[C:30]([C:32]([F:35])([F:34])[F:33])[CH:29]=[CH:28][C:27]=2[Cl:36])[CH:25]=1)=[O:20])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[C:7]([C:17]#[N:18])[CH:6]=1)C.[OH-].[Na+]>C(O)C>[Cl:36][C:27]1[CH:28]=[CH:29][C:30]([C:32]([F:34])([F:35])[F:33])=[CH:31][C:26]=1[N:24]1[CH:25]=[C:21]([C:19]([N:4]([C:5]2[CH:10]=[CH:9][C:8]([O:11][CH2:12][C:13]([CH3:15])([CH3:16])[CH3:14])=[C:7]([C:17]#[N:18])[CH:6]=2)[CH2:3][C:38]([OH:40])=[O:39])=[O:20])[C:22]([CH3:37])=[N:23]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 22227948HCID 22227948, Verbindung

Produkt 1

HCID 22228131HCID 22228131, VerbindungAusbeute 70,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Ethyl N-[1-(2-Chloro-5-trifluoromethylphenyl)-3-methylpyrazol-4-ylcarbonyl]-N-(3-cyano-4-neopentyloxyphenyl)glycine (1.8 g) was added to ethanol (15 ml). 10% aqueous sodium hydroxide solution (15 ml) was added and the mixture was stirred at a refluxing temperature for 30 min. The solvent was evaporated under reduced pressure, and dilute hydrochloric acid was added. The mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate, after which the solvent was evaporated under reduced pressure. A mixed solvent of chloroform-n-hexane was added to the residue to allow crystallization. The crystals were recrystallized from a mixed solvent of diisopropyl ether-n-hexane to give the title compound (1.2 g), melting point: 189–190° C.

Aufarbeitung

  1. customThe solvent was evaporated under reduced pressure, and dilute hydrochloric acid
  2. additionwas added
  3. extractionThe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customafter which the solvent was evaporated under reduced pressure
  7. additionA mixed solvent of chloroform-n-hexane was added to the residue
  8. customcrystallization
  9. customThe crystals were recrystallized from a mixed solvent of diisopropyl ether-n-hexane

Quellen und Nachweise

ORD-Eintrag
ord-82c5955f96514239927929bd123c00aa
Quelldatensatz
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07015218B1

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