Sodium Hydroxide → HCID 71257341, Verbindung

HRID 710097Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 710097
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([Br:8])=[CH:4][C:3]=1[OH:9].[F:10][C:11]1[CH:19]=[C:18]([S:20]([CH3:23])(=[O:22])=[O:21])[CH:17]=[CH:16][C:12]=1[C:13](O)=O.[OH-].[Na+]>>[Br:8][C:5]1[CH:6]=[CH:7][C:2]2[N:1]=[C:13]([C:12]3[CH:16]=[CH:17][C:18]([S:20]([CH3:23])(=[O:21])=[O:22])=[CH:19][C:11]=3[F:10])[O:9][C:3]=2[CH:4]=1

Komponenten

4

Edukt 3

HCID 14798Sodium HydroxideHCID 143206052-Amino-5-bromophenolHCID 283559322-Fluoro-4-(methylsulphonyl)benzoic acid

Produkt 1

HCID 71257341HCID 71257341, VerbindungAusbeute 13,2 %

Reaktionsbedingungen

Temperatur
195 °C

Versuchsvorschrift

2-amino-5-bromophenol (1.72 g, 9.2 mmol) and 2-fluoro-4-(methylsulfonyl)benzoic acid (2 g, 9.2 mmol) were dissolved in polyposphoric acid (30 g). This mixture was heated at 195° C. for three and half hours. Reaction mixture cooled to rt and diluted with ice water (100 ml). Aqueous layer basified with sodium hydroxide pellets to pH 9. Solid that formed was filtered and dried to obtain the crude. Crude was purified by combiflash using a gradient mixture of EtOAc and Petether (1:3) as eluent to afford the titled compound (450 mg) as a dark brown solid.

Aufarbeitung

  1. customReaction mixture
  2. temperaturecooled to rt
  3. customSolid that formed
  4. filtrationwas filtered
  5. customdried
  6. customto obtain the crude
  7. customCrude was purified by combiflash
  8. additiona gradient mixture of EtOAc and Petether (1:3) as eluent

Quellen und Nachweise

ORD-Eintrag
ord-7d032d3f32394817af7e648037b7de09
Quelldatensatz
uspto-grants-2015_11
Patentnummer
US09181214B2

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