Sulfuric Acid → HCID 86639059, Verbindung

HRID 1690056Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1690056
S(=O)(=O)(O)O.[F:6][C:7]([F:21])([F:20])[C:8]1[N:13]=[C:12]2[CH:14]=[C:15]([C:17]([OH:19])=[O:18])[NH:16][C:11]2=[CH:10][CH:9]=1>C(O)C>[F:21][C:7]([F:6])([F:20])[C:8]1[N:13]=[C:12]2[CH:14]=[CH:15][NH:16][C:11]2=[CH:10][CH:9]=1.[CH3:14][CH2:15][C:17]([O-:19])=[O:18]

Komponenten

4

Edukt 2

HCID 1118Sulfuric AcidHCID 573558695-(Trifluoromethyl)-1H-pyrrolo[3,2-b]pyridine-2-carboxylic acid

Produkt 1

HCID 86639059HCID 86639059, VerbindungAusbeute 168,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

1 mL (18.71 mmol) of concentrated sulfuric acid is added to a solution of 0.2 g (0.87 mmol) of 5-trifluoromethyl-pyrrolo[3,2-b]pyridine-2-carboxylic acid, obtained in Stage 10.2, in 10 mL of ethanol. It is stirred under reflux for 20 hours then the solution is cooled, and concentrated at reduced pressure. The resultant residue is then taken up in 50 mL of dichloromethane then washed successively with 20 mL of a saturated aqueous solution of sodium bicarbonate, 40 mL of water and 20 mL of saturated aqueous solution of sodium chloride, dried over sodium sulfate and then concentrated at reduced pressure. We obtain 0.19 g of product, which is used as it is in the next stage.

Aufarbeitung

  1. temperatureunder reflux for 20 hours
  2. temperaturethe solution is cooled
  3. concentrationconcentrated at reduced pressure
  4. washthen washed successively with 20 mL of a saturated aqueous solution of sodium bicarbonate, 40 mL of water and 20 mL of saturated aqueous solution of sodium chloride
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated at reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-b82352c8274a47799e4a9686a753c9ed
Quelldatensatz
uspto-grants-2012_04
Patentnummer
US08153650B2

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