反应详情

温度

0 °C

To a cooled (0° C.) stirring solution of (S)—N—((S)-(3-fluoropyridin-2-yl)(4-(trifluoromethyl)phenyl)methyl)-2-methylpropane-2-sulfinamide (108 g, 288.8 mmol) in DCM:EtOH (1:1,1080 mL), was added saturated HCl in 1,4-dioxane (216 mL). Stirring was continued for 2 h at 0° C. The progress of reaction was monitored by TLC (100% EtOAc). After completion of the reaction, the reaction mixture was concentrated and triturated with Et2O to give a white solid which was filtered and dried to give (S)-(3-fluoropyridin-2-yl)(4-(trifluoromethyl)phenyl) methanamine hydrochloride as a white solid. 1H-NMR (400 MHz, CDCl3) δ ppm 9.23 (s, 3H), 8.60 (d, J=4.8 Hz, 1H), 7.87 (d, J=1.2 Hz, 1H), 7.84 (d, J=8.4 Hz, 2H), 7.72 (d, J=8.4 Hz, 2H), 7.59-7.63 (m, 1H), 6.09 (s, 1H). MS (ESI pos. ion) m/z: 270.1 (M+H).

1. customThe progress of reaction
2. customAfter completion of the reaction
3. concentrationthe reaction mixture was concentrated
4. customtriturated with Et2O
5. customto give a white solid which
6. filtrationwas filtered
7. customdried