Sodium Hydroxide → HCID 58349828, Verbindung

HRID 1012521Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1012521
[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), a 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 the mixture was 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. extractionthe mixture was extracted 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-ba6f1592d3374e1283ffcb2a6e8187dc
Quelldatensatz
uspto-grants-2011_07
Patentnummer
US07977488B2

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