Hydrochloric Acid → 2-Amino-3,5-difluoro-6-(methylamino)pyridine

To a mixed solution of 10 ml of methanol and 1 ml of concentrated hydrochloric acid were added all amount of the above described 2-benzylamino-3,5-difluoro-6-(methylamino)pyridine together with 0.55 g of 10% palladium on carbon, and the mixture was hydrogenated at 50° C. overnight. The catalyst was separated by filtration, and the solvent and the like were distilled off under reduced pressure. To the residue was added 50 ml of chloroform, and the mixture was washed with 50 ml of 5% aqueous solution of sodium carbonate. The chloroform layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The solid precipitate was collected by filtration to obtain 840 mg of the title compound as a pale gray solid.

1. customThe catalyst was separated by filtration
2. distillationthe solvent and the like were distilled off under reduced pressure
3. additionTo the residue was added 50 ml of chloroform
4. washthe mixture was washed with 50 ml of 5% aqueous solution of sodium carbonate
5. dry with materialThe chloroform layer was dried over anhydrous magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. filtrationThe solid precipitate was collected by filtration

ORD-Eintrag

ord-2d4053268c764784bc29ab183101f678

Quelldatensatz

uspto-grants-2000_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06156903