Sodium Hydroxide → HCID 58349828, Verbindung

HRID 1426656Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1426656
[F:1][C:2]1[C:7]([C:8]2[N:12](S(C3C=CC=CC=3)(=O)=O)[CH:11]=[C:10]([CH:22]=[O:23])[CH:9]=2)=[CH:6][CH:5]=[CH:4][N:3]=1.[OH-].[Na+]>CO.O1CCCC1.[Cl-].[Na+].O>[F:1][C:2]1[C:7]([C:8]2[NH:12][CH:11]=[C:10]([CH:22]=[O:23])[CH:9]=2)=[CH:6][CH:5]=[CH:4][N:3]=1

Komponenten

6

Edukt 2

HCID 14798Sodium HydroxideHCID 866239745-(2-fluoropyridin-3-yl)-1-(phenylsulfonyl)-1H-pyrrole-3-carbaldehyde

Produkt 1

HCID 58349828HCID 58349828, VerbindungAusbeute 79,5 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittelHCID 57417360Sodium chloride; waterLösungsmittel

Versuchsvorschrift

5-(2-Fluoropyridin-3-yl)-1-(phenylsulfonyl)-1H-pyrrole-3-carbaldehyde (2.25 g) was dissolved in methanol (20 mL) and tetrahydrofuran (20 mL), 8 mol/L aqueous sodium hydroxide solution (20 mL) was added dropwise at room temperature and the mixture was stirred for 1 hr. The reaction mixture was diluted with saturated brine, and extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. Ethyl acetate was added to the residue, and insoluble crystals were collected by filtration to give the title compound as pale-brown crystals (yield 1.03 g, 79%).

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. additionEthyl acetate was added to the residue, and insoluble crystals
  6. filtrationwere collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-4f925fe412a94a6caa4ee4db78f380b3
Quelldatensatz
uspto-grants-2015_01
Patentnummer
US08933105B2

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