Triethylamine → HCID 59598232, Verbindung

To a solution of 1-(4-amino-3,5-difluoro-phenyl)-ethanone (2.35 g, 13.73 mmol) and Et3N (2 mL) in CH2Cl2 (10 mL) was added dropwise MsCl (2.34 mL, 2.34 mmol) at 0° C. The mixture was stirred for 3 hours at room temperature. The mixture was then diluted with EtOAc and 1N-HCl. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. The crude product was used directly in the following reaction. The crude residue was dissolved in THF (8 mL), after then was added 1N NaOH (4 mL) and CH3OH (4 mL) to the solution. After stirred for 5 hrs at room temperature, the mixture was diluted with EtOAc and 1N-HCl. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. The crude residue was purified by chromatography to afford N-(4-acetyl-2,6-difluoro-phenyl)-methanesulfonamide (1.85 g, 54%).

1. washThe organic layer was washed with water and brine
2. dry with materialdried over anhydrous magnesium sulfate
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe crude product was used directly in the following reaction
6. stirringAfter stirred for 5 hrs at room temperature
7. washThe organic layer was washed with water and brine
8. dry with materialdried over anhydrous magnesium sulfate
9. filtrationfiltered
10. concentrationconcentrated under reduced pressure
11. customThe crude residue was purified by chromatography

ORD-Eintrag

ord-a5f3a660cdc049cca209a73d048d5cdd

Quelldatensatz

uspto-grants-2010_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07858621B2