反应详情

A solution of Example 26B (142 mg, 0.7 mmol) and (R)-1-phenylethylamine (85 mg, 0.7 mmol) in absolute ethanol (1 mL) was stirred at 60° C. for 6 h. The mixture was concentrated under reduced pressure and purified by preparative HPLC on a Waters Symmetry C8 column (40 mm×100 mm, 7 μm particle size) using a gradient of 10% to 100% acetonitrile in 10 mM of ammonium acetate over 15 min at a flow rate of 70 mL/min to provide the title compound. MS (ESI+) m/z 277 (M+H)+; 1H NMR (300 MHz, DMSO-d6) δ ppm 1.46 (d, J=6.78 Hz, 3H) 2.28 (s, 3H) 3.83 (s, 2H) 5.10 (m, 1H) 6.95 (d, J=8.48 Hz, 1H) 7.16 (m, 3H) 7.29 (m, 1H) 7.35 (m, 5H) 9.37 (d, J=7.46 Hz, 1H).

1. concentrationThe mixture was concentrated under reduced pressure
2. custompurified by preparative HPLC on a Waters Symmetry C8 column (40 mm×100 mm, 7 μm particle size)
3. customover 15 min