反应详情

To a solution of cis-4-({[(1,1-dimethylethyl) oxy]carbonyl}amino)cyclohexanecarboxylic acid (3.0 g, 12 mmol, 1.0 equiv) and 1-[2-(trifluoromethyl)phenyl]methanamine (1.9 mL, 14 mmol, 1.0 equiv) in CH2Cl2 (82 mL) at room temperature, DMAP (301 mg, 2.47 mmol, 0.2 equiv) was added. EDC (2.95 g, 15.4 mmol, 1.25 equiv), and diisopropylethylamine (DIEA, 2.7 ml, 15 mmol, 1.25 equiv) were added. Stirring was continued overnight at room temperature. The solution was diluted with CH2Cl2 (100 ml), washed with saturated sodium bicarbonate (200 mL), water (200 mL), and brine (200 mL). The CH2Cl2 extracts were dried with MgSO4, filtered, and concentrated under reduced pressure to yield the title compound. MS (ES+): m/e 400.8 [M+Na]+.

1. washwashed with saturated sodium bicarbonate (200 mL), water (200 mL), and brine (200 mL)
2. dry with materialThe CH2Cl2 extracts were dried with MgSO4
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure