反应详情

Potassium carbonate (35 mg) and a 30% hydrogen peroxide solution (29 μl) were added to an ethanol (1 ml) solution containing (2R)-2-(5-cyano-3-fluoro-6-(quinolin-6-ylamino)pyridin-2-ylamino)-4-methylpentanamide (20 mg), followed by stirring at room temperature for 1 hour. A 30% hydrogen peroxide solution (29 μl) was added to the reaction mixture, followed by stirring at room temperature for 1 hour. Water, sodium chloride, and ethyl acetate were added to the reaction mixture. The organic layer was collected and dried over anhydrous magnesium sulfate, and the solvent was distilled away under reduced pressure. The obtained residue was dissolved in ethyl acetate, and diisopropylether was added. Solid matter was collected by filtration and washed with diisopropylether, and a yellow solid of 6-((2R)-1-amino-4-methyl-1-oxopentan-2-ylamino)-5-fluoro-2-(quinolin-6-ylamino)nicotinamide (8 mg) was thus obtained.

1. stirringby stirring at room temperature for 1 hour
2. customThe organic layer was collected
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationthe solvent was distilled away under reduced pressure
5. dissolutionThe obtained residue was dissolved in ethyl acetate
6. additiondiisopropylether was added
7. filtrationSolid matter was collected by filtration
8. washwashed with diisopropylether