反应详情

To a solution of 5-(2-aminoethyl)-N-[3-chloro-4-(3-chlorophenoxy)phenyl]-5H-pyrrolo[3,2-d]pyrimidin-4-amine dihydrochloride (200 mg), 2-(methylsulfonyl)acetic acid (113 mg) and 1-hydroxybenzotriazole (122 mg) in N,N-dimethylformamide (5.0 mL) were added a solution of triethylamine (419 mg) in N,N-dimethylformamide (1.25 mL) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (173 mg) under ice-cooling. After stirring the reaction mixture at room temperature for 16 hrs, water was added under ice-cooling, and the mixture was extracted twice with ethyl acetate. The organic layers were collected, dried over anhydrous magnesium sulfate and concentrated. The residue was purified by silica gel column chromatography (eluent:ethyl acetate/methanol=100/0→80/20), and recrystallized from ethanol-ethyl acetate-diisopropyl ether to give the title compound (151 mg) as crystals.

1. temperaturecooling
2. temperaturecooling
3. extractionthe mixture was extracted twice with ethyl acetate
4. customThe organic layers were collected
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated
7. customThe residue was purified by silica gel column chromatography (eluent:ethyl acetate/methanol=100/0→80/20)
8. customrecrystallized from ethanol-ethyl acetate-diisopropyl ether