反应详情

A mixture of Example 237 (68.5 mg, 0.146 mmol), cyclopropanecarboxylic acid (0.013 mL, 0.161 mmol), HOBT (26.9 mg, 0.176 mmol), EDC (33.7 mg, 0.176 mmol), and triethylamine (0.027 mL, 0.190 mmol) in DMF (2.5 mL) was stirred at room temperature overnight. More EDC (0.6 eq), HOBT (0.6 eq), acid (0.6 eq) and triethylamine (0.7 eq) were added. After 6 hours, water was added to reaction mixture. The precipitate was filtered and purified by reverse-phase HPLC as described in Example 56 to give the title compound (29.0 mg) as trifluoroacetic acid salts. 1H NMR (400 MHz, CD3OD) ppm 0.67-0.76 (m, 2H), 0.77-0.87 (m, 2H), 0.93-1.45 (m, 12H), 1.47-1.96 (m, 10H), 3.57 (m, 1H), 3.71 (m, 1H), 87 (m, 0.6H), 3.96 (s, 3H), 4.02 (m, 0.4H), 6.88-7.07 (m, 2H), 7.94 (m, 1H), 8.04 (s, 1H), 8.11 (s, 1H). MS (DCI+) m/z 536.4 (M+H)+.

1. filtrationThe precipitate was filtered
2. custompurified by reverse-phase HPLC