Phosphorus oxychloride → HCID 86659539, Verbindung

HRID 1256941Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1256941
[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:8](=O)[NH:7][CH:6]=[C:5]2[C:13]([O:15][CH3:16])=[O:14].P(Cl)(Cl)([Cl:19])=O>>[Cl:19][C:8]1[C:9]2[C:4](=[CH:3][C:2]([F:1])=[CH:11][CH:10]=2)[C:5]([C:13]([O:15][CH3:16])=[O:14])=[CH:6][N:7]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 53429435Methyl 6-fluoro-1-oxo-1,2-dihydroisoquinoline-4-carboxylate

Produkt 1

HCID 86659539HCID 86659539, Verbindung

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

To methyl 6-fluoro-1oxo-1,2-dihydroisoquinoline-4-carboxylate (756 mg), phosphoryl chloride (5 ml) was added, and the mixture was stirred at 100° C. for one hour. The resulting solution was returned to room temperature, and evaporated under reduced pressure to remove the solvent. To the resulting crude product, saturated sodium bicarbonate water was added, followed by extraction with ethyl acetate. The organic layer was washed with a saturated saline solution, dried over anhydrous magnesium sulfate, and evaporated under reduced pressure to remove the solvent to give methyl 1-chloro-6-fluoroisoquinoline-4-carboxylate (792 mg) as a brown solid.

Aufarbeitung

  1. customwas returned to room temperature
  2. customevaporated under reduced pressure
  3. customto remove the solvent
  4. additionTo the resulting crude product, saturated sodium bicarbonate water was added
  5. extractionfollowed by extraction with ethyl acetate
  6. washThe organic layer was washed with a saturated saline solution
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customevaporated under reduced pressure
  9. customto remove the solvent

Quellen und Nachweise

ORD-Eintrag
ord-046ac44e3bdc4c3d9c26c46413a558c1
Quelldatensatz
uspto-grants-2013_06
Patentnummer
US08461329B2

Notizen zur Reaktion

Wird geladen…