反应详情

An 87 μl portion of acetyl chloride and −170 μl of triethylamine were added to a mixture of 318 mg of 2-(2-aminoethylamino)-4-(3-methylanilino)pyrimidine-5-carboxamide and 20 ml of ethyl acetate, followed by stirring at room temperature for 30 minutes. Water and THF were added to the reaction mixture, followed by extraction with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and then concentrated under a reduced pressure. The resulting residue was recrystallized from a mixed solvent of THF and ethyl acetate, thereby obtaining 198 mg of 2-[(2-acetylaminoethyl)amino]-4-(3-methylanilino)pyrimidine-5-carboxamide (colorless crystals).

1. extractionfollowed by extraction with ethyl acetate
2. washThe organic layer was washed with saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated under a reduced pressure
5. customThe resulting residue was recrystallized from a mixed solvent of THF and ethyl acetate