반응 #56869
ord-dfdac2569fb948338d61c4cd647b18cd
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후처리
- 1기타Evaporation of the tetrahydrofuran
- 2여과under reduced pressure and filtration
실험 절차
To a stirred solution of 1-[4-(5-chloro-2-methyl-phenyl)-6-(4-trifluoromethyl-phenylamino)-pyrimidin-2-yl]-pyrrolidine-2,5-dione (0.15 g, 0.33 mmol), tetrahydrofuran (15 ml), and water (15 ml), cooled in an ice bath, was added aqueous sodium hydroxide solution (0.25 M, 4.0 ml, 1.0 mmol) dropwise. After stirring for 1 hour, hydrochloric acid (0.25 M, 8.0 ml, 2.0 mmol) was added dropwise. Evaporation of the tetrahydrofuran under reduced pressure and filtration provided the title compound as hydrochloride salt (93% yield). 1H NMR (CD3OD) δ 2.48 (s, 3H, CH3), 2.73-2.76 (m, 2H, CH2), 2.89-2.92 (m, 2H, CH2), 6.81 (s, 1H, Ar), 7.45 (d, 1H, J=8.3 Hz, Ar), 7.54 (dd, 1H, J=8.3 Hz, J=2.2 Hz, Ar), 7.60 (d, 1H, J=2.2 Hz, Ar), 7.76 (d, 2H, J=8.6 Hz, Ar), 8.04 (d, 2H, J=7.9 Hz, Ar).