反应详情

A mixture of the product of Example 1B (44.5 mg, 0.219 mmol), triethylamine (0.050 mL, 0.36 mmol), 2-(3,5-difluorophenyl)acetic acid (41.0 mg, 0.238 mmol), and O-(benzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium tetrafluoroborate (77.5 mg, 0.241 mmol) in DMF (0.75 mL) was stirred overnight, diluted with EtOAc, washed with 1 N NaOH and brine, dried (Na2SO4), and filtered. The residue was chromatographed on SiO2 (8% EtOAc/CH2Cl2) to give the title compound as a white solid (25.4 mg, 0.071 mmol). 1H NMR (300 MHz, DMSO-d6) δ 11.59 (s, 1H), 8.33 (dd, 1H), 8.16-8.09 (m, 1H), 8.00 (td, 1H), 7.89 (ddd, 1H), 7.19-7.07 (m, 3H), 3.75 (s, 2H), 3.61 (quin, 1H), 1.27 (d, 6H); MS (ESI+) M/Z 357.9 (M+H)+.

1. washwashed with 1 N NaOH and brine
2. dry with materialdried (Na2SO4)
3. filtrationfiltered
4. customThe residue was chromatographed on SiO2 (8% EtOAc/CH2Cl2)