Water → HCID 19956225, Verbindung

HRID 1779487Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1779487
P(Cl)(Cl)(Cl)=O.[CH3:6][C:7]1[CH:8]=[CH:9][C:10]([N:16]2[CH:20]=[CH:19][CH:18]=[CH:17]2)=[C:11]([CH:15]=1)[C:12]([OH:14])=O.O>CN(C)C=O>[CH3:6][C:7]1[CH:8]=[CH:9][C:10]2[N:16]3[CH:20]=[CH:19][CH:18]=[C:17]3[C:12](=[O:14])[C:11]=2[CH:15]=1

Komponenten

5

Edukt 3

HCID 962WaterHCID 24813Phosphorus oxychlorideHCID 149135585-Methyl-2-(1H-pyrrol-1-yl)benzoic acid

Produkt 1

HCID 19956225HCID 19956225, VerbindungAusbeute 35 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel2×

Versuchsvorschrift

At 0° C., add 1.36 ml (14.9 mmol) of phosphorus oxychloride to 1.14 ml (14.9 mmol) of dimethylformamide, then add a solution of 3 g (14.9 mmol) of 5-methyl-2-pyrrol-1-ylbenzoic acid (Preparation 25) in 30 ml of dimethylformamide. After one night's stirring at room temperature, hydrolyse the reaction mixture by pouring into 50 ml of water, extract with 200 ml of diethyl ether, and wash the ethereal phase in succession with water, a saturated aqueous hydrogen carbonate solution and then water. After drying over magnesium sulfate and rendering colourless with animal charcoal, the ethereal phase is concentrated to dryness to yield the title compound.

Aufarbeitung

  1. extractionextract with 200 ml of diethyl ether
  2. washwash the ethereal phase in succession with water
  3. dry with materialAfter drying over magnesium sulfate and rendering colourless with animal charcoal
  4. concentrationthe ethereal phase is concentrated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-386a5f86a788485f86c1969127f186a0
Quelldatensatz
uspto-grants-1997_05
Patentnummer
US05627203

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