反应详情

温度

25 °C

A solution containing the product from Example 3D (0.025 g, 0.055 mmol) in DMF (0.5 mL) was treated with the product from Example 3L (0.021 g, 0.056 mmol), EDAC (0.020 g, 0.104 mmol), HOBT (0.015 g, 0.111 mmol), and NMM (0.020 mL, 0.182 mmol) at 0° C., stirred at 25° C. for 16 hours, and partitioned between ethyl acetate and water. The organic phase was washed with 10% citric acid, diluted sodium bicarbonate, and brine, dried over MgSO4, filtered and concentrated. The residue was purified by reversed phase chromatography on a C18 column, eluting with 5-100% acetonitrile in water (0.1% TFA) to give the title compound (0.028 g, 63% yield). 1H NMR (300 MHz, DMSO-d6), δ ppm 0.79 (m, 15 H), 0.95 (m, 1 H), 1.29 (m, 1 H), 1.49 (m, 2 H), 1.80 (m, 1 H), 2.68 (m, 4 H), 3.03 (m, 1 H), 3.17(m, 2 H), 3.55 (s, 3 H), 3.63 (m, 3 H), 3.94 (d, J=11.03 Hz, 2 H), 4.12 (m, 2 H), 4.47 (m, 2 H), 6.62 (d, J=9.93 Hz, 1 H), 7.07 (m, 10 H), 7.25 (d, J=9.56 Hz, 1 H), 7.48 (m, 1 H), 7.57 (s, 1 H), 7.75 (d, J=8.46 Hz, 1 H), 7.93 (m, 1 H), 8.10 (d, J=8.09 Hz, 1 H), 8.62 (d, J=4.04 Hz, 1 H).

1. custompartitioned between ethyl acetate and water
2. washThe organic phase was washed with 10% citric acid, diluted sodium bicarbonate, and brine
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified by reversed phase chromatography on a C18 column
7. washeluting with 5-100% acetonitrile in water (0.1% TFA)