Dichloromethane → HCID 22493592, Verbindung

In 100 ml of dichloromethane were dissolved 4.2 g of methyl 8-isopropylquinolone-2-carboxylate, 3 ml of 2,6-lutidine and 209 mg of 4-dimethylaminopyridine under a nitrogen gas stream. Trifluoromethanesulfonic anhydride (3.2 ml) was added dropwise to the resulting solution at 0° C., followed by stirring at room temperature for 24 hours. A saturated aqueous solution of ammonium chloride was added to the reaction mixture and the resulting mixture was extracted with dichloromethane. The organic layer was successively washed with water and saturated saline, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue so obtained was subjected to chromatography on a silica gel column (developing solvent: 5% ethyl acetate/n-hexane), whereby 6.3 g of the title compound were obtained in the form of a colorless solid.

1. extractionthe resulting mixture was extracted with dichloromethane
2. washThe organic layer was successively washed with water and saturated saline
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue so obtained

ORD-Eintrag

ord-de60dbd62761450b851e4433bf8b163c

Quelldatensatz

uspto-grants-2003_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06630463B2