反应详情

温度

100 °C

A mixture of (3S)-8-amino-9,10-difluoro-2,3-dihydro-3-methyl-7-oxo-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carbonitrile (702 mg, 2.53 mmol), trans-3-(1H-pyrazol-1-yl)cyclopentylamine (460 mg, 3.04 mmol) and di-isopropylethylamine (0.970 mL, 5.57 mmol) in anhydrous DMSO (14 mL) was stirred at 100° C. for 7 h. After cooling, the reaction mixture was poured into ice-water and then extracted with CH2Cl2-MeOH. The organic layer was washed with water and brine, and dried over anhyd Na2SO4 followed by the removal of solvent. The crude product was purified by column chromatography (Hexane/EtOAc=1/10→EtOAc) to yield (3S)-8-amino-9-fluoro-2,3-dihydro-3-methyl-7-oxo-10-[trans-3-(1H-pyrazol-1-yl)cyclopentylamino]-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carbonitrile (108 mg, 10%) as a yellow powder.

1. temperatureAfter cooling
2. extractionextracted with CH2Cl2-MeOH
3. washThe organic layer was washed with water and brine
4. dry with materialdried over anhyd Na2SO4
5. customfollowed by the removal of solvent
6. customThe crude product was purified by column chromatography (Hexane/EtOAc=1/10→EtOAc)