反应详情

(S)-1-(5-chloropyridin-2-yl)-1-(3-fluoro-5-(trifluoromethyl)phenyl)-2-phenylethanamine (0.15 g, 0.38 mmol) was dissolved in dichloromethane (5 mL) at room temperature. Solid powdered K2CO3 (0.52 g, 3.8 mmol) was added followed by 4-nitrophenyl carbonochloridate (0.11 g, 0.56 mmol). The resulting slurry was stirred at room temperature for 14 h, diluted with DCM (ca. 50 mL) and washed with sat. NaHCO3 (ca. 4×20 mL). The organic portion was dried over anhydrous Na2SO4, decanted and concentrated yielding (S)-4-nitrophenyl 1-(5-chloropyridin-2-yl)-1-(3-fluoro-5-(trifluoromethyl)phenyl)-2-phenylethylcarbamate as a pale brown oil, (0.20 g, crude quantitative yield). LCMS: 2.26 min [M+1] 560.2 (2 min gradient, MeOH/H2O 0.1% TFA)

1. washwashed with sat. NaHCO3 (ca. 4×20 mL)
2. dry with materialThe organic portion was dried over anhydrous Na2SO4
3. customdecanted
4. concentrationconcentrated