反应详情

A mixture of the product of Example 11B (40.3 mg, 0.18 mmol), triethylamine (0.037 mL, 0.26 mmol), 2-(3,5-difluorophenyl)acetic acid (36.4 mg, 0.21 mmol), and O-(benzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium tetrafluoroborate (61.8 mg, 0.19 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 (3% EtOAc/CH2Cl2) to give the title compound as a white solid (4.8 mg, 0.013 mmol). 1H NMR (300 MHz, DMSO-d6) δ 11.95 (s, 1H), 8.44 (d, 1H), 8.23-7.90 (m, 3H), 7.26-7.00 (m, 3H), 3.80 (s, 2H); MS (DCI) M/Z 401.2 (M+NH4)+.

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