反应详情

A mixture of 5-(2-aminoethyl)-N-{3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}-5H-pyrrolo[3,2-d]pyrimidin-4-amine dihydrochloride (150 mg), 2-(methylsulfonyl)acetic acid (79.6 mg), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (166 mg), 1-hydroxybenzotriazole monohydrate (133 mg), triethylamine (0.40 mL) and N,N-dimethylformamide (5.0 mL) was stirred at room temperature for 20 hrs. Water was added to the reaction system and the mixture was extracted with ethyl acetate. The organic layer washed with water and saturated brine and dried over magnesium sulfate. After concentration under reduced pressure, the residue was separated and purified by basic silica gel column chromatography (eluent, ethyl acetate→ethyl acetate:methanol=4:1). Crystallization from ethyl acetate-diisopropyl ether gave the title compound (128 mg) as colorless powder crystals.

1. extractionthe mixture was extracted with ethyl acetate
2. washThe organic layer washed with water and saturated brine
3. dry with materialdried over magnesium sulfate
4. concentrationAfter concentration under reduced pressure
5. customthe residue was separated
6. custompurified by basic silica gel column chromatography (eluent, ethyl acetate→ethyl acetate:methanol=4:1)
7. customCrystallization from ethyl acetate-diisopropyl ether